反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 1,1-dimethylethyl 2-{4-[(dimethylamino)carbonyl]phenyl}-4,5,7,8-tetrahydropyrazolo[3,4-d]azepine-6(2H)-carboxylate (may be prepared as described in Description 41) (194 mg, 0.50 mmol) in dichloromethane (14 ml) was added trifluoroacetic acid (7 ml). The resulting mixture was stirred at room temperature, under argon, for 2 hours and then diluted with methanol. Reaction was purified by SCX, eluting with methanol and then 2M ammonia/methanol. The basic fractions were combined and solvent evaporated in vacuo. Resulting crude product was purified further by column chromatography on silica gel, eluting with a mixture of 2M ammonia in methanol/dichloromethane (0-3%) to afford the title compound (D42). MS (ES+) m/e 285 [M+H]+.
WORKUP
后处理
- customReaction
- customwas purified by SCX
- washeluting with methanol
- customsolvent evaporated in vacuo
- customResulting crude product
- customwas purified further by column chromatography on silica gel
- washeluting with a mixture of 2M ammonia in methanol/dichloromethane (0-3%)