반응 #65119

반응 방정식

(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

용매

dichloromethane

반응 조건

후처리

1. 1
   기타evaporated to dryness
2. 2
   workup.DISSOLUTIONThe residue was dissolved in toluene
3. 3
   기타the solution again evaporated to dryness
4. 4
   workup.DISSOLUTIONthe residue dissolved in dichloromethane
5. 5
   세척The solution was washed with saturated aqueous sodium carbonate solution, with water and with saturated brine
6. 6
   건조dried over sodium sulphate
7. 7
   기타evaporated to dryness

실험 절차

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.

출처