反応 #65119

反応方程式

(2β,3α,5α,16β)-3-hydroxy-2,16-di-(1-piperidinyl)-androstan-17-one

acetylchloride

→

(2β,3α,5α,16β)-3-acetyloxy-2,16-di-(1-piperidinyl)androstan-17-one

溶媒

dichloromethane

反応条件

後処理

1. 1
   その他evaporated to dryness
2. 2
   workup.DISSOLUTIONThe residue was dissolved in toluene
3. 3
   その他the solution again evaporated to dryness
4. 4
   workup.DISSOLUTIONthe residue dissolved in dichloromethane
5. 5
   洗浄The solution was washed with saturated aqueous sodium carbonate solution, with water and with saturated brine
6. 6
   乾燥dried over sodium sulphate
7. 7
   その他evaporated to dryness

実験手順

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.

出典