反应详情

A flask is charged with nicotinic acid (5.0 g, 40.6 mmol). Thionyl chloride (30.0 mL) is added and the reaction is refluxed for 1 h. It is then cooled to room temperature and concentrated in vacuo. The residue is dissolved in anhydrous dichloromethane (30 mL) and O,N-dimethyl-hydroxylamine (4.35 g, 44.0 mmol) is added, followed by addition of triethylamine (14.15 g, 100.0 mmol). The reaction mixture is stirred at room temperature for 1.5 h. It is then washed with water and the aqueous phase is extracted with dichloromethane. The combined organic layer is dried over sodium sulfate and concentrated in vacuo to afford N-methyl-N-methoxy-nicotinamide as a brown oil. MS (ESI) m/z 167.0 (M+H)+.

1. temperaturethe reaction is refluxed for 1 h
2. concentrationconcentrated in vacuo
3. dissolutionThe residue is dissolved in anhydrous dichloromethane (30 mL)
4. washIt is then washed with water
5. extractionthe aqueous phase is extracted with dichloromethane
6. dry with materialThe combined organic layer is dried over sodium sulfate
7. concentrationconcentrated in vacuo