HRID256816

反应详情

EQUATION

反应方程式

HRID 256816 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 40 g (0.119 mole) of BOC-CYCLOHEXYLGLYCINE, O,N-DIMETHYLHYDROXAMIDE in 550 ml Et2O was cooled in ice and 148 ml (0.148 mole) of a 1M solution of LiAlH4 in Et2O added over 0.5 hour. After an additional 15 minutes, the mixture was treated cautiously with 28 g of KHSO4 in 100 ml H2O. The mixture was filtered through Celite and washed with 10% citric acid and saturated NaHCO3. After drying the solvent was removed under reduced pressure to give the crude BOC-CYCLOHEXYLGLYCINAL. The material was used immediately in the following reaction. ##STR175##

WORKUP

后处理

  1. filtrationThe mixture was filtered through Celite
  2. washwashed with 10% citric acid and saturated NaHCO3
  3. customAfter drying the solvent
  4. customwas removed under reduced pressure