HRID36841

反应详情

EQUATION

反应方程式

HRID 36841 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 40 g of (2β,3α,5α,16β)-3-hydroxy-2,16-di-(1-piperidinyl)-androstan-17-one in 160 ml of dichloromethane were added 13.5 ml of acetylchloride at 15°-20 ° C. The solution was stirred for 6 h at room temperature and thereafter evaporated to dryness. The residue was dissolved in toluene, the solution again evaporated to dryness and the residue dissolved in dichloromethane. The solution was washed with saturated aqueous sodium carbonate solution, with water and with saturated brine, dried over sodium sulphate, and evaporated to dryness to give 43.5 g of (2β,3α,5α,16β)-3-acetyloxy-2,16-di-(1-piperidinyl)androstan-17-one. Mp 154° C.

WORKUP

后处理

  1. customevaporated to dryness
  2. dissolutionThe residue was dissolved in toluene
  3. customthe solution again evaporated to dryness
  4. dissolutionthe residue dissolved in dichloromethane
  5. washThe solution was washed with saturated aqueous sodium carbonate solution, with water and with saturated brine
  6. dry with materialdried over sodium sulphate
  7. customevaporated to dryness