反应详情

A solution of 3-methoxy-4-nitrobenzoic acid (6.81 g, 34.54 mmol) in sulfurous dichloride (50 mL) was stirred at reflux for 8 hours. After cooling to ambient temperature, the mixture was concentrated under vacuum and the residue was dissolved in dichloromethane (60 mL). 1-Methylpiperazine (3.6 g, 36.27 mmol) was added at 0° C. and the mixture was stirred at ambient temperature for 4 hours. The mixture was poured into water (100 mL) and extracted with dichloromethane (2×200 mL). The organic phase was dried over anhydrous sodium sulfate, filtered and concentrated to provide the crude title compound. MS: 280.2 (M+H+).

1. temperatureat reflux for 8 hours
2. concentrationthe mixture was concentrated under vacuum
3. dissolutionthe residue was dissolved in dichloromethane (60 mL)
4. extractionextracted with dichloromethane (2×200 mL)
5. dry with materialThe organic phase was dried over anhydrous sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated