反应详情

4-Ethylhexanoic acid (47.0 g) was dissolved in DMF (190 mL). To the solution were added piperidine (34.0 mL), HOBt.H2O (52.7 g) and WSC.HCl (66.1 g). The mixture was stirred at RT overnight. To the reaction mixture were added ethyl acetate (300 mL) and 1 N hydrochloric acid (100 mL) at ice temperature. The aqueous layer was removed and the organic layer was washed with saturated aqueous sodium bicarbonate (150 mL×2) and brine (100 mL×2), then dried over sodium sulfate. The sodium sulfate was filtered off and the filtrate was concentrated in vacuo to give the title compound (59.8 g) as a crude product.

1. customThe aqueous layer was removed
2. washthe organic layer was washed with saturated aqueous sodium bicarbonate (150 mL×2) and brine (100 mL×2)
3. dry with materialdried over sodium sulfate
4. filtrationThe sodium sulfate was filtered off
5. concentrationthe filtrate was concentrated in vacuo