反応 #156649

反応方程式

TMEDA

sec-butyllithium

THF

4-chloro-piperidine-1-carboxylic acid tert-butyl ester

THF

→

2-Aza-bicyclo[3.1.0]hexane-2-carboxylic acid tert-butyl ester

溶媒

water

Ethyl acetate

反応条件

後処理

1. 1
   workup.STIRRINGThe reaction mixture was stirred for 2 h at −78° C.
2. 2
   その他to return slowly to room temperature
3. 3
   抽出the aqueous phase was extracted several times with ethyl acetate
4. 4
   乾燥dried over sodium sulfate
5. 5
   その他the solvent was removed in vacuum

実験手順

TMEDA (0.11 mL) was slowly added dropwise at −78° C. to a mixture of sec-butyllithium (1.4 M; 0.52 mL) and THF (1.8 mL). Then it was stirred for a further 30 min at −78° C. and then a solution of 4-chloro-piperidine-1-carboxylic acid tert-butyl ester (160 mg) in a little THF was slowly added dropwise. The reaction mixture was stirred for 2 h at −78° C., then it was allowed to return slowly to room temperature. Ethyl acetate and water were added to the reaction mixture and the aqueous phase was extracted several times with ethyl acetate. The organic phases were combined, dried over sodium sulfate and the solvent was removed in vacuum.

出典