With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.4045-44-7,1,2,3,4,5-Pentamethylcyclopenta-1,3-diene,as a common compound, the synthetic route is as follows.
Under an argon atmosphere the excess of 1,2,3,4,5-pentamethylcyclopentadiene(19 mL, 0.167 mmol) was added to the suspensionof [(C8H14)2RhCl]2 (30 mg, 0.084 mmol) in C2H4Cl2 (1 ml).The reaction mixture was stirred overnight at room temperature.Then, the excess of NaHCO3 (84 mg, 1.00 mmol) was added and themixture was cooled to 0 C in an ice bath. The solution of bromine(135 mg, 43 mL, 0.84 mmol) in C2H4Cl2 (0.5 ml)was added dropwise.After the addition, the reaction mixture was stirred for another30 min at 0 C. The mixture was then opened to air and filtered, theprecipitate was washed with C2H4Cl2 (4 1 ml) and the combinedsolution was evaporated in vacuum. The precipitate (presumably[Cp*RhBr3]n) was washed with Et2O (32 ml) and dried in vacuum(20 mg, 50%). The obtained precipitate was suspended in hot C2H4Cl2 (3 ml)and ethylene was bubbled through until the complete dissolutionof the precipitate. The mixture was evaporated to dryness in vacuum.The residue was dissolved in CHCl3 (1 ml) and the product 3was precipitated by Et2O (5 ml) as red powder, which was dried invacuum (16 mg, 94%).1H NMR (400 MHz, CDCl3): delta 1.73 (s, 15H). 13C NMR (101 MHz,CDCl3): delta 94.98 (d, JRh-C 8.8 Hz), 10.15. Anal. Calc. forC10H15RhBr2: C 30.18, H 3.80; found: C 30.58, H 3.98., 4045-44-7
As the paragraph descriping shows that 4045-44-7 is playing an increasingly important role.
Reference£º
Article; Pototskiy, Roman A.; Lisov, Alexey A.; Nelyubina, Yulia V.; Perekalin, Dmitry S.; Journal of Organometallic Chemistry; vol. 862; (2018); p. 71 – 75;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI