反应详情

温度

65 °C

After adding 1.88 g (4.07 mmoles) of 2,4-bis(1-adamantylamino)-6-(1-piperazinyl)pyrimidine and 0.56 g of potassium carbonate to a solution containing 2.00 g (3.57 mmoles) of 21-(4-bromobenzenesulfonyloxy)-16α-methylpregna-1,4,9(11)-triene-3,20-dione in 100 ml of acetonitrile, the reaction mixture is stirred at a temperature of 65° C. for 5 hours, then evaporated. The residue is distributed between 40 ml of chloroform and 10 ml of water. After separation the chloroform layer is dried and evaporated. The residue is purified by chromatography on a silica gel column by using a 98:2 mixture of chloroform/methanol as eluent. After recrystallization from ether the title compound is obtained in a yield of 2.48 g (88.5%), m.p.:210°-220° C.

1. customevaporated
2. customAfter separation the chloroform layer
3. customis dried
4. customevaporated
5. customThe residue is purified by chromatography on a silica gel column
6. additiona 98:2 mixture of chloroform/methanol as eluent
7. customAfter recrystallization from ether the title compound
8. customis obtained in a yield of 2.48 g (88.5%), m.p.:210°-220° C.