HRID220103

反应详情

EQUATION

反应方程式

HRID 220103 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

16.5 g of (±)-3,4-bis-cyclopropylmethoxy-N-[(3RS,4RS)-4-(3,4-dimethoxyphenyl)-7-oxabicyclo[4.1.0]-hept-3-yl]benzamide (compound E1) are dissolved in 500 ml of tert-butanol, 5.0 g of sodium borohydride are added and the reaction mixture is heated to boiling. After slow addition of 70 ml of methanol, the reaction mixture is cooled and treated with 200 ml of water and 150 ml of ethyl acetate. The organic phase is dried using sodium sulfate, concentrated and the residue is chromatographed on silica gel using a mixture of petroleum ether/ethyl acetate in the ratio 1/2. 11.3 g of the title compound are obtained.

WORKUP

后处理

  1. temperaturethe reaction mixture is heated to boiling
  2. temperaturethe reaction mixture is cooled
  3. customThe organic phase is dried
  4. concentrationconcentrated
  5. customthe residue is chromatographed on silica gel using
  6. additiona mixture of petroleum ether/ethyl acetate in the ratio 1/2