反应 #3095953
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09315446B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Polidocanol 41.32 g (70.9 mmol) Polidocanol, 21.07 g (178.4 mmol) ethyl lactate, 4.64 g Novozyme 435 and 1.00 g (11.9 mmol) sodium bicarbonate were added to a 100 mL 1-neck round bottom flask. The flask was then fitted to a rotary evaporator with the bath temperature set at 62° C. The pressure was slowly reduced to 15 mmHg under moderate rotation and the reaction mixture was held for 8 hours. Ethyl lactate (5.79 g, 49.0 mmol) was added to replenish the amount removed by distillation and the mixture was held an additional 16 hours at 62° C. and 15 mmHg. The round bottom flask was removed from the evaporator and the mixture was diluted with 20 mL petroleum ether. The solids were separated by vacuum filtration on a Buchner funnel with a #1 Whatman filter paper. The filtered solids were washed with 16 mL petroleum ether and the wash liquors were combined with the mother liquors. The combined filtrates were added to a 100 mL 1-neck round bottom flask and the flask was affixed to a rotary evaporator. The petroleum ether and excess ethyl lactate were distilled @15 mmHg with a bath temperature of 75-80° C. Upon completion of the distillation the pot was cooled and 38.19 g of Polidocanol lactate was obtained as a lightly colored waxy solid. The flask was then fitted to a rotary evaporator with the bath temperature set at 62° C removed by distillation the mixture was held an additional 16 hours at 62° C. The round bottom flask was removed from the evaporator the mixture was diluted with 20 mL petroleum ether The solids were separated by vacuum filtration on a Buchner funnel with a #1 Whatman filter paper The filtered solids were washed with 16 mL petroleum ether The combined filtrates were added to a 100 mL 1-neck round bottom flask the flask was affixed to a rotary evaporator The petroleum ether and excess ethyl lactate were distilled @15 mmHg with a bath temperature of 75-80° C Upon completion of the distillation the pot was cooled
来源 ID: ord-5b9ef8e7f74042c98d3e8bca876aa261