HRID429335

反应详情

EQUATION

反应方程式

HRID 429335 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

232 g of compound 3 are dissolved in 500 ml of ethanol. Cool in ice-bath and add 100 g of sodium borohydride in 500 ml of water. Stir for 2 hours. Add acetic acid until the sodium borohydride has been neutralized. Cool the solution in ice-bath under an atmosphere of nitrogen and add 10 g of 10% Pd/C catalyst. Stir under a hydrogen atmosphere at 15PSI until the reaction is complete, as judged by TLC. Filter through celite and evaporate organic solvents. Extract with ethyl acetate. Dry over sodium sulfate. Filter. Evaporate solvent.

WORKUP

后处理

  1. temperatureCool in ice-bath
  2. temperatureCool the solution in ice-bath under an atmosphere of nitrogen
  3. stirringStir under a hydrogen atmosphere at 15PSI until the reaction
  4. filtrationFilter through celite
  5. customevaporate organic solvents
  6. extractionExtract with ethyl acetate
  7. dry with materialDry over sodium sulfate
  8. filtrationFilter