62937-45-5,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.
Methyl /so-butyl ketone (MIBK; 3.87 ml/g of mandelic acid) was added to the mandelic acid (1 eq.) at ambient temperature. Stirring was started and the solution was heated to 80C. A solution of D-prolinamide (0.5 eq.) in MIBK (0.43 ml/g of mandelic acid) and water (3 molar equivalent/mandelic acid) was added and crystallisation started soon after. After half an hour additional MIBK (3.87 ml/g of mandelic acid) was added and then a solution of D-prolinamide (0.7 eq.) in MIBK (0.43 ml/g of mandelic acid) and water (3 molar equivalent/mandelic acid). The suspension was stirred at 100C for 22 hours. The suspension was cooled to O0C over 2.25 hours. The substance was isolated by filtration, washed with MIBK and then dried (crude yield 84.9 %). The ee of the crude D-prolinamide salt of the (i?)-enantiomer of the mandelic acid was 94.32%. If the optical purity and the assay of the salt are not satisfactory, a series of slurry wash experiments in a number of solvents has shown that both the optical purity and the assay (physical content purity) can be improved. A slurry wash in acetone, for example, gave the (R)- mandelic acid.D-prolinamide salt with 99.1% ee. The yield including the slurry wash was 81.8%. With 2-butanone (MEK) as solvent for the slurry wash, the (i?)-mandelic acid.D- prolinamide salt was obtained with 96.0% ee in 83.9% yield. Other solvents or solvent mixtures which can be used for the slurry wash are MIBK with 20 % w/w H2O, acetonitrile, and 2- propanol.
As the paragraph descriping shows that 62937-45-5 is playing an increasingly important role.
Reference£º
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2006/125964; (2006); A1;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI