HRID267146

反应详情

EQUATION

反应方程式

HRID 267146 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1.1 g of 1-(benzyloxycarbonyl)-4-(tert.butoxycarbonyl)-N-tert.butyl-2-piperazinecarboxamide were dissolved in 40 ml of ethanol. 0.1 g of 10% palladium-on-carbon was added and the mixture was hydrogenated at room temperature and under atmospheric pressure for 2 hours. The catalyst was filtered off. The filtrate was evaporated to give 0.74 g of crude product which was purified by flash chromatography on silica gel using 5% methanol in dichloromethane for the elution. After evaporation of the solvents there was obtained 0.44 g of 4-(tert.butoxycarbonyl)-N-tert.butyl-2-piperazinecarboxamide as an oil; MS: m/e 286 [M+H]+.

WORKUP

后处理

  1. filtrationThe catalyst was filtered off
  2. customThe filtrate was evaporated
  3. customto give 0.74 g of crude product which
  4. customwas purified by flash chromatography on silica gel using 5% methanol in dichloromethane for the elution
  5. customAfter evaporation of the solvents