反应详情

After adding 1.40 g (4.57 moles) of 2,4-bis(1,1-dimethylethylamino)-6-(1-piperazinyl}pyrimidine and 0.63 g of potassium carbonate to a solution containing 2.00 g (3.805 mmoles) of 21-(4-nitrobenzenesulfonyloxy)-16α-methylpregna-1,4,9(11)-triene-3,20-dione in 100 ml of acetone, the reaction mixture is boiled under reflux for 8.5 hours, then evaporated. The residue is distributed between 40 ml of chloroform and 10 ml of water. The chloroform layer is dried and evaporated. The residue is purified on a silica gel column by using a 98:2 mixture of chloroform/methanol as eluent. After recrystallization the title compound is obtained in a yield of 1.53 g (64%), m.p.:145°-155° C.

1. temperatureunder reflux for 8.5 hours
2. customevaporated
3. dry with materialThe chloroform layer is dried
4. customevaporated
5. customThe residue is purified on a silica gel column
6. additiona 98:2 mixture of chloroform/methanol as eluent
7. customAfter recrystallization the title compound
8. customis obtained in a yield of 1.53 g (64%), m.p.:145°-155° C.