反応 #4814
ord-61f54da028b24a72bc1f764a9ad4f9e4
反応方程式
溶媒
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1その他The resulting mixture was evaporated in vacuo
- 2温度After cooling
- 3その他the reaction mixture was triturated with ether
- 4その他separated by filtration
- 5その他Recrystallization from dichloromethane
- 6その他dioxane gave 4.2 g (0.012 mol), 65%, 9, mp 199°-201°
実験手順
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.