反应详情

温度

57.5 °C

3.80 g (20.9 mmol) dimethylamino-pentanoic acid were added to 25 ml thionyl chloride and stirred for 90 min. at 55-60° C. The remaining thionyl chloride was distilled in vacuum and the residue was added to a solution of 2.00 g (9.42 mmol) 2-phenylamino-benzamide (see above) in 30 ml trichloromethane at 0° C. The reaction mixture was boiled for 4 h and stirred overnight at room temperature. The residue was filtrated and dissolved in dichloromethane and saturated sodium bicarbonate solution. The organic solvent was dried over magnesium sulfate and evaporated. The yellow oil slowly crystallized.

1. distillationThe remaining thionyl chloride was distilled in vacuum
2. waitThe reaction mixture was boiled for 4 h
3. stirringstirred overnight at room temperature
4. filtrationThe residue was filtrated
5. dissolutiondissolved in dichloromethane
6. dry with materialThe organic solvent was dried over magnesium sulfate
7. customevaporated
8. customThe yellow oil slowly crystallized