反应详情

温度

5 °C

Intermediate 40 (400 mg, 1.87 mmol) was dissolved in glacial acetic acid (20 ml) and 17% HCl (10 ml). This solution was cooled to 5° C. and a solution of sodium nitrite (260 mg, 3.74 mmol) in water (5 ml) was added slowly during 10 min. The reaction was stirred for 1 h at 5° C. The reaction mixture was then added to a saturated solution of sulfur dioxide (generated from sodium sulfite and conc. HCl) in acetic acid: benzene (3:2) containing cupric chloride dihydrate (100 mg, 0.513 mmol). The reaction was sired at room temperature for 20 h and then poured water (500 ml) and extracted with ethyl acetate (3×100 ml). The extract was washed with water (5×100 ml) and dried over anhydrous sodium sulfate. The solvent was evaporated to give the product as brown solid (350 mg) which was directly used to make the sulfonamide.

1. waitThe reaction was sired at room temperature for 20 h
2. extractionpoured water (500 ml) and extracted with ethyl acetate (3×100 ml)
3. washThe extract was washed with water (5×100 ml)
4. dry with materialdried over anhydrous sodium sulfate
5. customThe solvent was evaporated