反応 #468578

反応方程式

ditertiarybutylcarbonate

4-piperidone monohydrate hydrochloride salt

sodium hydroxide

→

N-t-butyloxycarbonyl-4-piperidone

収率 40.0%

溶媒

Water

反応条件

後処理

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

実験手順

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.

出典