反应详情

Combine methyl 2-methoxy-5-methylsulfonamidobenzoate (1.0 g, 3.86 mmol) and lithium hydroxide (93 mg, 3.86 mmol) in tetrahydrofuran/water (50 mL/10 mL). After 18 hours, add lithium hydroxide (100 mg) and heat to reflux. After 1 hour, cool to ambient temperature and evaporate to remove most of the tetrahydrofuran. Dilute the evaporated reaction mixture with water (about 70 mL) and acidify to pH of about 1 using a 1 M aqueous hydrochloric acid solution. Evaporate to dryness and triturate with dichloromethane (200 mL). Filter and evaporate the filtrate to give the title compound: mp; 160-163° C.

1. temperatureheat to reflux
2. waitAfter 1 hour
3. customevaporate
4. customto remove most of the tetrahydrofuran
5. additionDilute
6. customthe evaporated reaction mixture with water (about 70 mL)
7. customEvaporate to dryness
8. customtriturate with dichloromethane (200 mL)
9. filtrationFilter
10. customevaporate the filtrate