反应 #4814

ord-61f54da028b24a72bc1f764a9ad4f9e4

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The resulting mixture was evaporated in vacuo
  2. 2
    温度After cooling
  3. 3
    其他the reaction mixture was triturated with ether
  4. 4
    其他separated by filtration
  5. 5
    其他Recrystallization from dichloromethane
  6. 6
    其他dioxane gave 4.2 g (0.012 mol), 65%, 9, mp 199°-201°

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04727151uspto-grants-1988_02