反应详情

4,4-Dimethylvaleric acid (348 g), piperidine (291 mL) and DMF (1.7 L) were mixed. To the mixture were added HOBt.H2O (450 g) and WSC.HCl (563 g) at ice temperature. After the mixture was stirred at RT overnight, water (1.7 L) was added to the reaction mixture at ice temperature and the mixture was extracted with toluene (500 mL, and 400 mL×2). The organic layer was washed with aqueous 10 w/v % sodium carbonate (1 L) and water (1 L), then concentrated in vacuo to give the title compound (508 g) as a crude product.

1. extractionthe mixture was extracted with toluene (500 mL, and 400 mL×2)
2. washThe organic layer was washed with aqueous 10 w/v % sodium carbonate (1 L) and water (1 L)
3. concentrationconcentrated in vacuo