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 (9.51 mmol) 4,5-Dimethoxy-2-methylamino-benzamide (see above) dissolved in 30 ml trichloromethane at 0° C. The mixture was boiled for 4 h. After filtration the residue was dissolved in trichloromethane and saturated sodium bicarbonate solution. The organic solution was dried over magnesium sulfate and evaporated under vacuum.

1. distillationThe remaining thionyl chloride was distilled in vacuum
2. waitThe mixture was boiled for 4 h
3. filtrationAfter filtration the residue
4. dissolutionwas dissolved in trichloromethane
5. dry with materialThe organic solution was dried over magnesium sulfate
6. customevaporated under vacuum