Tag: M.W:100-200

13910-48-0, N1-Benzylpropane-1,3-diamine is a catalyst-ligand compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

2-(4-tert-butylphenyl) -4-(methylsulfanyl) -6H,7H-pyrazolo [1,5 -aj [1,3 ,5j triazin-7 -one(75 mg, 0.239 mmol) and (3-aminopropyl)(benzyl)amine (117 mg, 0.71 mmol) were dissolved in Pyridine (1 mL). The reaction mixture was heated in a microwave at 140 C for2h. The reaction mixture was evaporated to dryness and purified by preparative HPLC method A affording the title compound as a pale yellow oil (35 mg, 34 %).?H NMR (500 MHz, Methanol-d4) 8.36 (s, 2H), 8.29 – 8.20 (m, 2H), 7.56 – 7.46(m, 2H), 7.44 -7.30 (m, 5H), 5.70 (s, 1H), 4.15 (s, 2H), 3.83 (t, I = 6.3 Hz, 2H), 3.24 -3.08 (m, 2H), 2.18 (dt, I = 14.2, 6.5 Hz, 2H), 1.37 (s, 9H). LCMS Method B: ft 2.44 mm, 100 %; m/z 432 (MH)., 13910-48-0

The synthetic route of 13910-48-0 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; PRESIDENT AND FELLOWS OF HARVARD COLLEGE; EVOTEC INTERNATIONAL GMBH; GAMPE, Christian, M.; KAHNE, Daniel, Evan; KAHNE, Suzanne, Walker; QIAO, Yuan; EAST, Stephen; PARKES, Alastair, L.; SOUTHEY, Michelle; HUNTER, James; WHITTAKER, Mark; ARTHUIS, Martin; (359 pag.)WO2016/191658; (2016); A1;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.62937-45-5,D-Prolinamide,as a common compound, the synthetic route is as follows.

62937-45-5, In these Reference Examples the following method was used, with volumes and amounts as outlined in Table 1.The racemic mandelic acid derivative 3-chloro,5-difluoro-methoxy mandelic acid and (D)- proline amide were added to ethyl acetate saturated in water (8.1% water in ethyl acetate). The mixture was heated to reflux and stirred for 10 minutes at reflux. The thin suspension was cooled to 23C over 13 hours followed by further cooling to 180C over 40 minutes. The suspension was filtered and washed with ethyl acetate (3 x 30 ml) to give the salt. A sample was dissolved in a 1 : 1 mixture of 1 M HCl and ethyl acetate. The organic layer was separated, concentrated to dryness and analysed by chiral HPLC (for suitable methodology, see Reference Example 1 IA). This showed a high degree of purity of the “correct” enantiomer (see Table 1), (R)- 3-chloro,5-difluoro-methoxy mandelic acid.Table 1MA= racemic mandelic acid derivative, 3-chloro,5-difluoro-methoxy mandelic acid.PA= (D)-proline amide.Eq. PA= Amount of equivalents of (D)-proline amide compared to racemic mandelic acid derivative.EtOAc= ethyl acetate, as solution saturated in water.Water/EtOAc (%) = concentration of water in ethyl acetate. mmol MA/ ml water-EtOAc= concentration range of racemic mandelic acid derivative per ml of ethyl acetate and water. EPO e.e. (%) = enantiomeric excess defined as the % mole fraction denoting the enantiomers in a mixture.1) Corrected for purity, i.e. initially 86% pure racemic mandelic acid derivative.; In these Reference Examples the following method was used, with volumes and amounts as outlined in Table 2.The racemic mandelic acid derivative 3-chloro,5-difluoro-methoxy mandelic acid and (D)- proline amide were added to ethyl acetate and the mixture heated to reflux. At reflux, water was added and the mixture was stirred for another 10 minutes at reflux. The thin suspension was allowed to cool to 18C over 3 hours (in Reference Examples 4-8; 4 hours in Reference Example 9). The suspension was filtered and washed with ethyl acetate (3 x 30 ml) to give the salt. The salt was dissolved in a 1 : 1 mixture of 1 M HCl and ethyl acetate. The organic layer was separated, concentrated to dryness and analysed by chiral HPLC (for suitable methodology, see Reference Example 1 IA). This showed a high degree of purity of the “correct” enantiomer (see Table 2), (R)- 3-chloro,5-difluoro-methoxy mandelic acid.To exemplify in more detail, the following scheme was used in Reference Example 6: The racemic mandelic acid derivative 3-chloro,5-difluoro-methoxy mandelic acid (26.18 g, 93.3 mmol, 1 eq, 90% pure according to HPLC) and (D)-proline amide (4.80 g, 42 mmol, 0.45 eq) were added to ethyl acetate (54.5 ml) and the mixture heated to reflux. At reflux, 5.5 ml of water was added and the mixture stirred for another 10 minutes at reflux. The thin suspension was allowed to cool to 18C over 3 hours. The suspension was filtered and washed with ethyl acetate (3 x 30 ml) to give 8.6 g of the salt. A sample was dissolved in a 1:1 mixture of 1 M HCl and ethyl acetate. The organic layer was separated, concentrated to dryness and analysed by chiral HPLC. This showed 98.2% of the “correct” (i?)-enantiomer. From the mother liquor more material crystallised, which was filtered, washed and dried. This gave another 1.6 g of the salt. The free (i?)-mandelic acid was analysed by HPLC (for suitable methodology, see Reference Example HA) and contained 99.0% of the “correct” enantiomer. EPO Table 2MA = racemic mandelic acid derivative 3-chloro,5-difluoro-methoxy mandelic acid.PA = (D)-proline amide.Eq. PA = Amount of equivalents of proline amide compared to racemic mandelic acid derivativeEtOAc = ethyl acetate in ml.Water/EtOAc (%) = concentration of water in ethyl acetate. mmol MA/ ml water-EtOAc = concentration range of racemic mandelic acid derivative per ml of ethyl acetate and water. e.e. (%) = enantiomeric excess defined as the % mole fraction denoting the enantiomers in a mixture.1) Corrected for purity, i.e. initially 85-90% pure racemic mandelic acid derivative.2) The suspension was allowed to cool to 180C over 4 hours.; A solution of the racemic mandelic acid (obtained after the first racemisation) in ethyl o acetate (1.433 kg of a 29.9% (w/w) solution, 0.429 kg racemic mandelic acid, 1.698 mol, 1.00 eq) was filtered and added within 30 minutes to a stirred solution of D-prolinamide (0.095 kg, 0.853 mol, 0.49 eq) in ethyl acetate (0.407 kg, 0.452 L) as well as water (0.153 kg) at 72-75C. After the addition was completed a clear solution was obtained. The mixture was cooled to 58C within 45 min. No crystallisation was observed. The mixture s was cooled further to 0-20C within 2.5 hours. The salt started to precipitate at approximately 55C. After stirring for a further hour at 0-20C, the solid was filtered off and washed twice with a pre-cooled (0-50C) mixture of ethyl acetate/ water = 9:1 (w/w, 2 x EPO 0.20 kg). A wet,…

62937-45-5 D-Prolinamide 447554, acatalyst-ligand compound, is more and more widely used in various fields.

Reference£º
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2006/125964; (2006); A1;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

4730-54-5, 1,4,7-Triazacyclononane is a catalyst-ligand compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A three necked flask was charged with TACN (5.0 g, 39 mmol), followed by the additionof deoxygenated ethanol (150 mL), LiOHH2O (0.4 g, 9.5 mmol) in deoxygenated H2O (50 mL).The resulting solution was slightly cloudy and was allowed to stir at 50 C for 30 min. 4-Vinylbenzylchloride (1.1 g, 7.5 mmol) in ethanol was added dropwise to the mixture. The reaction mixture wasrefluxed under N2. After 2 h, the reaction mixture was concentrated to 50 mL on a rotary evaporator.Water was added to the residue and the solution was extracted 3-times with dichloromethane (30 mL).The combined dichloromethane extracts were washed with brine, dried with anhydrous Na2SO4,and concentrated under reduced pressure. The residue was loaded onto a silica column and elutedusing chloroform-methanol (50:50, v/v, and 1% of triethylamine). Upon removal of the solvents,the chromatographically purified N-(4-vinylbenzyl)-1,4,7-triaza-cyclononane (0.5 g) was obtainedas a light brown viscous oil and used immediately for the preparation of the grafted polystyreneparticles. Typical recovered yields of the purified N-(4-vinylbenzyl)-1,4,7-triaza-cyclononane were5%, 1H-NMR (CDCl3), delta (ppm), 2.65-3.1 (m, 12H, ring CH2) 3.68 (s, 2H, benzyl CH2), 5.18 (d, 1H,CH=CH2), 5.65 (d, 1H, CH=CH2), 6.65 (dd, 1H, CH=CH2), 7.20 (d, 2H, aromatic CH), 7.30 (d, 2H,aromatic CH), FT-IR (KBr) 3361, 2918, 2849, 1654, 1559 cm-1.

4730-54-5, The synthetic route of 4730-54-5 has been constantly updated, and we look forward to future research findings.

Reference£º
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

767-60-2, 3-Methyl-1H-indene is a catalyst-ligand compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

(6/5-tert-Butyl-2-methyl-1H-inden-4/7-yl)(cyclopenta-2,4-dien-1-yl)dimethylsilane To a solution of 971 mg (13.5 mmol) of CpLi in 100 ml of THF a solution of 3.77 g (13.5 mmol) of chloro(dimethyl)(2-methyl-5-tert-buthyl-1H-inden-7-yl)silane in 10 ml of THF was added dropwise by vigorous stirring for 5 min at -80 C. This mixture was additionally stirred for 1 h at room temperature, and 1 ml of water was added. The mixture was evaporated to dryness, and 100 ml of water was added to the residue. The crude product was extracted with 3*50 ml of dichloromethane. The combined organic extract was dried over Na2SO4 and evaporated to dryness. The product was isolated from the residue by flash chromatography using a short column with Silica Gel 60 (40-63 um, d 60 mm, l 50 mm; eluent: hexanes). Yield 3.85 g (86%) of pure cyclopenta-2,4-dien-1-yl(dimethyl)(2-methyl-5-tert-buthyl-1H-inden-7-yl)silane. Anal. calc. for C21H28Si: C, 81.75; H, 9.15. Found: C, 81.52; H, 9.09. 1H NMR (CDCl3): delta 7.35-7.39 (m, 2H, 4,6-H in indenyl), 6.65 (br.s, 2H, 3,4-H in Cp), 6.50-6.56 (m, 3H, 3-H in indenyl and 2,5-H in Cp), 3.78 (br.s, 1H, 1-H in Cp), 3.36 (s, 2H, 1,1′-H in indenyl), 2.19 (s, 3H, 2-Me in indenyl), 1.39 (s, 9H, C(CH3)3 in indenyl), 0.25 (s, 6H, SiMe2). 13C{1H} NMR (CDCl3): delta 148.6, 145.9, 145.7, 145.4, 133.5 (br.), 131.7, 130.6 (br.), 127.3, 126.2, 118.3, 51.1, 43.7, 31.6, 29.7, 16.8, -3.5.Complex 22-Zr (0413) (0414) To a solution of 3.73 g (10.0 mmol) of (6/5-tert-butyl-2-methyl-1H-inden-4/7-yl)(dimethyl)(3-methyl-1H-inden-1-yl)silane in 200 ml of ether 8.0 ml of 2.5 M (20 mmol) of n-BuLi in hexanes was added by vigorous stirring for 5 min at room temperature. This mixture was stirred for 12 h, then cooled to -30 C., and 3.77 g (10 mmol) of ZrCl4(THF)2. The resulting mixture was stirred for 24 h at room temperature and then evaporated to dryness. A mixture of the residue obtained and 200 ml of toluene was stirred for 6 h at 80 C. and then filtered through glass frit (G4). The precipitate was additionally washed by 3¡Á50 ml of hot toluene. The combined extract was evaporated to dryness, and the residue was re-crystallized from 30 ml of toluene. Crystals precipitated at -30 C. were collected, washed by 3¡Á4 ml of cold toluene, 2¡Á7 ml of hexanes, and dried in vacuum. Yield 2.61 g (49%) of one pure isomer. (0415) Anal. calc. for C26H30Cl2SiZr: C, 58.62; H, 5.68. Found: C, 58.89; H, 5.79. (0416) 1H NMR (CD2Cl2): delta 7.35-7.40 (m, 3H, 5,7-H in 2-methylindenyl and 4-H in 3-methylindenyl), 7.10 (m, 1H, 5-H in 3-methylinden-1-yl), 6.88 (m, 1H, 6-H in 3-methylinden-1-yl), 6.75 (d, J=7.6 Hz, 7-H in 3-methylindenyl) 6.48 (m, 1H, 3-H in 2-methylindenyl), 6.45 (m, 1H, 1-H in 2-methylindenyl), 6.27 (m, 1H, 2-H in 3-methylindenyl), 2.49 (s, 3H, Me in 3-methylinden-1-yl), 2.24 (s, 3H, Me in 2-methylinden), 1.34 (s, 9H, 5-C(CH3)3 in 2-methylindenyl), 1.02 (s, 3H, SiMeMe?), 0.89 (s, 3H, SiMeMe?). (0417) 13C{1H} NMR (CD2Cl2): delta 149.9, 139.7, 133.8, 132.1, 131.3, 129.3, 127.0, 126.6, 126.4, 126.1, 125.8, 123.5, 121.0, 119.3, 117.4, 108.7, 99.2, 98.9, 34.8, 30.6, 16.8, 13.7, -1.9, -4.0.

767-60-2, As the paragraph descriping shows that 767-60-2 is playing an increasingly important role.

Reference£º
Patent; Borealis Technology Oy; Voskoboynik, Alexander Zelmanovich; Asachenko, Andrei Fyodorovich; Konanovich, Dmitry; Nikulin, Mikhail V.; Tzarev, Alexey; Maaranen, Janne; Vanne, Tiina; Kauhanen, Jyrki; Mansner, Erik; Kokko, Esa; Saarinen, Laura; US8569532; (2013); B2;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

4062-60-6,4062-60-6, N1,N2-Di-tert-butylethane-1,2-diamine is a catalyst-ligand compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A suspension of 30.1 mg (3-isobutyryl-6-methoxy-lH-indazol-l-yl)acetic acid in 1 mL DCM was treated with 38 muL oxalyl chloride and 10 muL DMF at room temperature for 2.5 hours. The reaction mixture was evaporated to dryness and the residue taken up in 1 mL dry DCM and treated with 8.6 mg N^-di-tert-butylethane-l^-diamine and 15 muL triethylamine over night. Purification of the reaction mixture on RP-etaPLC afforded the title compound following lyophilization. LC-MS: 4.19 min. (m/Z: 711.5, 689.5, 577.4, 633.5).

The synthetic route of 4062-60-6 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; MERCK & CO., INC.; WO2008/30390; (2008); A2;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

62937-45-5, D-Prolinamide is a catalyst-ligand compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

62937-45-5, (R)-chloro[(1,2,3,4,5-eta)-pentamethyl-2,4-cyclopentadien-1-y 1](2-pyrrolidinecarboxamidato-kappaN1, kappaN2)iridium(III) (Cp*Ir(Cl-) (R-PA-H+)) To 40 ml of methylene chloride, 1.593 g of a pentamethylcyclopentadienyl iridium(III) chloride dimer ([Cp*IrCl2]2), 502 mg of (R)-prolinamide and 425 mg of triethylamine were successively added, and the mixture was continuously stirred at room temperature overnight. To the reaction mixture, 10 ml of a 20% aqueous sodium chloride solution was added, and the mixture was stirred for about 30 minutes and then left to stand. The resulting layers were separated. The aqueous layer was extracted with 10 ml of methylene chloride, and then the organic layers were combined and washed with 10 ml of a 20% aqueous sodium chloride solution. Further, this aqueous layer was extracted with 10 ml of methylene chloride, and then the organic layers were combined and dried over 10 g of anhydrous sodium sulfate overnight. The desiccant was filtered off and washed with methylene chloride, and then the filtrate was concentrated in vacuo. To the concentrated residue, 20 ml of tetrahydrofuran/diisopropyl ether (1/1) was added, and the mixture was stirred at 35 to 40C for about 1 hour. The precipitate was collected by suction filtration, washed with 10 ml of tetrahydrofuran/diisopropyl ether (1/1), and then dried in vacuo at 40 to 50C for 5 hours to give 1.813 g of (R)-chloro[(1,2,3,4,5-eta)-pentamethyl-2,4-cyclopentadien-1-y 1](2-pyrrolidinecarboxamidato-kappaN1, kappaN2)iridium(III) (Cp*Ir(Cl-)(R-PA-H+)) as a yellow crystalline powder. Melting point: 174.8C Elemental analysis: C15H24ClIrN2O (476.01) calculated value (%) C37.84, H5.08, N5.88, Ir40.4 found value (%) C37.81, H5.07, N5.93, Ir40.7 IR (KBr): 3429, 3282, 1599 cm-1 1H-NMR (200 MHz, CDCl3) : delta 1.60-2.28 (4H, m, 2 * CH2), 1.70 (15H, s, 5Me of Cp*), 2.71-2.93 (1H, m, one of NCH2), 3.41-3.55 (1H, m, one of NCH2), 3.89-4.01 (1H, m, NCH), 4.96 (2H, br, 2 * NH). 13C-NMR (50.3 MHz, CDCl3) : delta 9.1 (5Me of Cp*), 27.1 (CH2), 28.2 (CH2), 54.3 (NCH2), 62.9 (NCH), 84.4 (ArC of Cp*), 183.5 (C=O).

As the paragraph descriping shows that 62937-45-5 is playing an increasingly important role.

Reference£º
Patent; Hamari Chemicals, Ltd.; MAEDA, Sadayuki; SATO, Tatsunori; KAWANO, Yasuhiko; MIYAWAKI, Toshio; EP2733138; (2014); A1;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.4411-80-7,6,6′-Dimethyl-2,2′-bipyridine,as a common compound, the synthetic route is as follows.

General procedure: To a solution of [{M(mu-Cl)(ptpy)2}2] (M=Rh, Ir) (0.15mmol) in 25mL of a mixture of CH2Cl2/MeOH/H2O (1:1:0.5) the bipyridine ligand (0.3mmol) was added and the mixture refluxed with stirring for 3h. After cooling to room temperature KPF6 (0.5mmol) was added and stirred for 20min. The solvent was removed to dryness in vacuo and the residue dissolved in dichloromethane and chromatographed on alumina with CH2Cl2/acetone (9:1) as the eluent. The resulting solution was evaporated to dryness and the residue was redissolved in 5ml of dichloromethane and the product was precipitated by slow diffusion of isohexane.

4411-80-7, The synthetic route of 4411-80-7 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Graf, Marion; Gothe, Yvonne; Siegmund, Daniel; Metzler-Nolte, Nils; Suenkel, Karlheinz; Inorganica Chimica Acta; vol. 471; (2018); p. 265 – 271;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

294-90-6, 1,4,7,10-Tetraazacyclododecane is a catalyst-ligand compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,294-90-6

To a 100 mL round bottom flask fitted with a reflux condenser and stir bar was added 1.4696 g Cyclen (8.5 mmol). 5.44 11 g of 2-bromoacetamide (39.4 mmol, 4.6 eq) was added with 4.5748 g triethylamine (44.9 mmol, 5.3 eq) in 30 mL absolute ethanol. The contents were refluxed for 4 hours at 80 C, after which time a white precipitate formed in the flask. After cooling to room temperature, the precipitate was decanted and placed in a 250 mL round bottom flask, then dissolved in 200 mL of hot 80 % ethanol/20 % water. The volume was reduced by approximately 30 % on a roto-evaporator, then placed in the refrigerator overnight to produce white crystals. The remaining solvent was removed by filtration and the crystals were transferred to a 50 mL round bottom flask to dry on a Schlenk line under vacuum for several hours (66 % yield). ESI-MS: m/z = 401.3 (100 %), 402.3 (15 %) [M + H]+; 423.4 (25 %), 424.4 (< 10 %) [M + Na]+. 1H NMR (500 MHz, D20), ppm: 3.02 (s, amide pendent CH28H), 2.57 (s, Cyclen ring 16 H). 13C NMR (125 MHz, D20), ppm: 174.07 (carbonyl C),55.86 (amide CH2), 50.42 (ring CH2). As the paragraph descriping shows that 294-90-6 is playing an increasingly important role. Reference£º
Patent; THE RESEARCH FOUNDATION FOR THE STATE UNIVERSITY OF NEW YORK UNIVERSITY AT BUFFALO; HEALTH RESEARCH, INC.; MORROW, Janet, R.; TSITOVICH, Pavel, B.; DORAZIO, Sarina, J.; OLATUNDE, Abiola, O.; SNYDER, Eric, M.; SPERNYAK, Joseph, A.; BURNS, Patrick; BOND, Christopher, J.; WO2015/38943; (2015); A1;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

13093-04-4, N1,N6-Dimethylhexane-1,6-diamine is a catalyst-ligand compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a four-neck 2000 mL RBF fitted with overhead stirrer, addition funnel, reflux condenser, and thermocouple, under N2, was added maleic anhydride (75g, 0.734 mol, 2.5 eq.) and dry acetonitrile (400 mL), followed by the dropwise addition of N,N’-dimethyl-1,6-hexanediamine (51.9 mL, 0.294 mol, 1 eq.), maintaining <30C. The reaction turned an orange color as the addition progressed. The reaction was heated to 450C for 2 hours, then stirred overnight at room temperature. By morning, a tan solid had precipitated. It was filtered, then dried to constant weight, giving 87.6 g (87%) of the desired product as an off-white solid. 13093-04-4, As the paragraph descriping shows that 13093-04-4 is playing an increasingly important role.

Reference£º
Patent; E. I. DU PONT DE NEMOURS AND COMPANY; WO2006/66031; (2006); A1;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.6249-56-5,3-Carboxy-N,N,N-trimethylpropan-1-aminium chloride,as a common compound, the synthetic route is as follows.

6249-56-5, Example 620-Oxo-5p-pregnan-3a-yl 4-(trimethylammonium) butanoate chloride3-Carboxy-N,N,N-trimethylpropan-l -ammonium chloride (prepared according to Lindstedt and Lindstedt, 1965, 69 mg; 0.38 mmol) was suspended in anhydrous CH2C12 (1 mL) under argon. The reaction flask was cooled in ice bath and oxalyl chloride (0.5 mL; 5.82 mmol) was added dropwise, followed by catalytic amount of dry DMF (3 mu; 0.03 mmol). The heterogeneous mixture was then brought to r.t. and stirred for 16 hrs, during which all the solids dissolved. The mixture was evaporated under the reduced pressure and solid residue was dissolved in dry nitromethane (2 mL) and dry pyridine (0.10 mL; 1.24 mmol) under argon. Compound II (100 mg; 0.31 mmol) was added to this reaction mixture, which was then stirred for 4 hrs. Reaction was quenched with water (10 mL) and acidified to pH 4 with 5percent aq. HC1. Product was extracted with CHC13 (3 x 20 mL), solution was washed with brine (10 mL, dried with anhydrous MgS04 and evaporated under the reduced pressure. Trituration with benzene removed the unreacted starting steroide II and the remaining product was subsequently crystallized from CHC13 : n-heptane (1 : 1) to give needle-like crystals (134 mg; 89percent).[a]D = +88.4 (c 0.243); NMR (500 MHz, CDC13) delta 4.76-4.68 (m, 1H, 3-CH), 3.73-3.73 (bm, 2H, 4′-CH2), 3.47 (s, 9H, NCH3), 2.55 (t, 1H, J = 9.0 Hz, 17-CH), 2.49 (t, 2H, J = 6.2 Hz, 2′-CH2), 2.12 (s, 3H, 21- CH3), 0.94 (s, 3H, 19-CH3), 0.60 (s, 3H, 18-CH3). 13C NMR (101 MHz, CDC13) delta 209.47, 171.49, 75.20, 65.61, 63.79, 56.62, 53.45, 44.26, 41.83, 40.41, 39.13, 35.76, 34.96, 34.59, 32.19, 31.46, 30.27, 26.87, 26.59, 26.24, 24.37, 23.22, 22.89, 20.82, 18.46, 13.38.IR (CHC13): 2956 (NMe3+), 1722 (C=0, ester), 1699 (C=0, ketone), 1478 (NMe3+) 1386 (CH3), 1360(COCH3), 1230 (NMe3+), 1188 (CO), cm”1.ESI m/z 446.6 (100percent, [M-C1]+); HRMS-ESI m/z 446.3624 ([M-C1]+, C28H4803N requires 446.3629).For C28H48C1N03 (482,1) calculated: 69.75percent C; 10.03percent H, 7.35percent CI, 2.91percent N; found: 69.59percent C, 9.99percent H, 7.12 percent CI, 2.82percent N.

6249-56-5 3-Carboxy-N,N,N-trimethylpropan-1-aminium chloride 22620, acatalyst-ligand compound, is more and more widely used in various fields.

Reference£º
Patent; USTAV ORGANICKE CHEMIE A BIOCHEMIE AKADEMIE V?D ?ESKE REPUBLIKY, V.V.I.; FYZIOLOGICKY USTAV AKADEMIE V?D ?ESKE REPUBLIKY, V.V.I.; CHODOUNSKA, Hana; KAPRAS, Vojt?ch; VYKLICKY, Ladislav; BOROVSKA, Ji?ina; VYKLICKY, Vojt?ch; VALE?, Karel; STUCHLIK, Ale?; RAMBOUSEK, Luka?; WO2012/110010; (2012); A1;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI