反应详情

温度

0 °C

To a solution of (2S)-2-(tert-butoxycarbonylamino)-N-[2-[4-(4-chlorophenyl)-1-piperazinyl]-2-oxoethyl]-3-(2-pyridyl)-propanamide (42 g) in methanol (84 ml) was added 4N hydrogen chloride in ethyl acetate (209 ml) at 0° C. and the mixture was stirred at 0° C. for 30 minutes. The reaction mixture was allowed to warm to room temperature, stirred for 2 hours and diluted with ethyl acetate. The resulting solid was collected by filtration and washed with ethyl acetate. The solid was poured into aqueous sodium hydrogencarbonate solution and the mixture was extracted with chloroform. The aqueous layer was extracted twice with chloroform. The combined organic layers were dried over sodium sulfate and concentrated in vacuo to give a crude product of the title compound (27 g).

1. temperatureto warm to room temperature
2. stirringstirred for 2 hours
3. filtrationThe resulting solid was collected by filtration
4. washwashed with ethyl acetate
5. additionThe solid was poured into aqueous sodium hydrogencarbonate solution
6. extractionthe mixture was extracted with chloroform
7. extractionThe aqueous layer was extracted twice with chloroform
8. dry with materialThe combined organic layers were dried over sodium sulfate
9. concentrationconcentrated in vacuo