반응 #468578

반응 방정식

ditertiarybutylcarbonate

4-piperidone monohydrate hydrochloride salt

sodium hydroxide

→

N-t-butyloxycarbonyl-4-piperidone

수율 40.0%

용매

Water

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   온도under cooling on ice
3. 3
   workup.STIRRINGthe mixture was vigorously stirred for 6 hours at room temperature
4. 4
   추출The reaction mixture was subjected to extraction with ethyl acetate
5. 5
   기타the extract was evaporated to dryness under reduced pressure
6. 6
   기타to thereby yield a pale yellow solid
7. 7
   기타By recrystallization of the solid from hexane

실험 절차

Water (250 ml) was added to 4-piperidone monohydrate hydrochloride salt (75 g) for dissolution, and 1 N aqueous solution of sodium hydroxide (1000 ml) was added thereto. To the solution, ditertiarybutylcarbonate (120 g) was added dropwise with stirring under cooling on ice, and the mixture was vigorously stirred for 6 hours at room temperature. The reaction mixture was subjected to extraction with ethyl acetate, and the extract was evaporated to dryness under reduced pressure to thereby yield a pale yellow solid. By recrystallization of the solid from hexane, N-t-butyloxycarbonyl-4-piperidone (3) (38.9 g) was obtained in the form of white needle-shaped crystals.

출처