反应详情

After adding 7.9 g of triethylamine to a solution containing 9 g of 2β-(4-hydroxy-1-piperidinyl)-16β-(1-pyrrolidinyl)-5α-androstane-3α,17β-diol in 80 ml of methylene chloride, 9 g of acetyl chloride are dropwise added to the solution at a temperature of 0° C. under cooling and stirring. After termination of the addition, the reaction mixture is maintained at room temperature for 24 hours. After completion of the reaction the excess of acetyl chloride is decomposed by water, the methylene chloride solution is washed with aqueous sodium hydroxide solution until it becomes acid-free, then washed with water several times until neutral. After drying the methylene chloride solution and evaporating, the residue is purified on a silica gel column to yield 8.3 g (71.9%) of the title compound, Rf1 =0.36.

1. additionare dropwise added to the solution at a temperature of 0° C.
2. temperatureunder cooling
3. additionAfter termination of the addition
4. washthe methylene chloride solution is washed with aqueous sodium hydroxide solution until it
5. washwashed with water several times until neutral
6. dry with materialAfter drying the methylene chloride solution
7. customevaporating
8. customthe residue is purified on a silica gel column