HRID4718

反应详情

EQUATION

反应方程式

HRID 4718 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To an ether solution of benzoyl chloride 2.81 g (0.02 mol) there was added dropwise 1.67 g (0.02 mol) 1-methylimidazole with stirring. The resulting mixture was evaporated in vacuo and the residue was allowed to react with 2.12 g (0.02 mol) benzaldehyde at 70° overnite. After cooling, the reaction mixture was triturated with ether and was solid separated by filtration. Recrystallization from dichloromethane:dioxane gave 4.2 g (0.012 mol), 65%, 9, mp 199°-201°; ir (KBr) 1740 cm-1 ; pmr (CDCl3) δ 4.17 (s, 3H), 8.18-7.25 (m, 12H), 8.50 (s, 1H) and 11.1 (bs, 1H) ppm.

WORKUP

后处理

  1. customThe resulting mixture was evaporated in vacuo
  2. temperatureAfter cooling
  3. customthe reaction mixture was triturated with ether
  4. customseparated by filtration
  5. customRecrystallization from dichloromethane
  6. customdioxane gave 4.2 g (0.012 mol), 65%, 9, mp 199°-201°