HRID621207
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
A solution of 1,2,3,9-tetrahydro-9-methyl-3-[[5-methyl(triphenylmethyl)-1H-imidazol-4-yl]methyl]carbazol-4-one (268 mg) in a mixture of glacial acetic acid (5 ml), THF (5 ml), and water (5 ml) was heated at 100°-110° for 8 h. After cooling, 2N sodium hydroxide solution (50 ml) was added and the resulting suspension was extracted with dichloromethane (2×50 ml). The combined, dried organic extracts were concentrated to give a foam which was purified by FCC eluting with System A (100:8:1) to give the title compound (114 mg) as a solid. The 1H-n.m.r. and t.l.c. of this material were consistent with those obtained for the product of Example 8.
WORKUP
后处理
- temperaturewas heated at 100°-110° for 8 h
- temperatureAfter cooling
- extractionthe resulting suspension was extracted with dichloromethane (2×50 ml)
- concentrationdried organic extracts were concentrated
- customto give a foam which
- customwas purified by FCC
- washeluting with System A (100:8:1)