反应详情

温度

65 °C

After adding 1.88 g (4.07 moles) 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 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 solution is dried, evaporated and the residue is purified by chromatography on a silica gel column. A 98:2 mixture of chloroform/methanol is used for elution and the product obtained is recrystallized from ether to give the title compound in a yield of 2.48 g (88.5%), m.p.: 210°-220° C.

1. customevaporated
2. customAfter separation the chloroform solution
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
7. washis used for elution
8. customthe product obtained
9. customis recrystallized from ether