HRID621207

反应详情

EQUATION

反应方程式

HRID 621207 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturewas heated at 100°-110° for 8 h
  2. temperatureAfter cooling
  3. extractionthe resulting suspension was extracted with dichloromethane (2×50 ml)
  4. concentrationdried organic extracts were concentrated
  5. customto give a foam which
  6. customwas purified by FCC
  7. washeluting with System A (100:8:1)