تفاعل #65119

معادلة التفاعل

(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

المذيبات

dichloromethane

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر