Reacción #65119

ord-bd8175091f0e4c5691795727be49dd1c

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

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

Procedimiento

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.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05418226uspto-grants-1995_05