反应详情

Thionyl chloride (3.7 g) was added dropwise under ice cooling to a solution of 5.0 g (33 mmol) of 3,5-diaminobenzoic acid in 250 ml of methanol, followed by stirring at room temperature for 2 hours and then stirring under heating and reflux for additional 6 hours. After the solvent was distilled out under reduced pressure, the residue was neutralized with aqueous ammonia and then extracted with methylene chloride. The extract was dried over sodium sulfate and then dried up under reduced pressure, whereby 3.3 g of white powder were obtained (yield: 60%).

1. stirringstirring
2. temperatureunder heating
3. temperaturereflux for additional 6 hours
4. distillationAfter the solvent was distilled out under reduced pressure
5. extractionextracted with methylene chloride
6. dry with materialThe extract was dried over sodium sulfate
7. customdried up under reduced pressure