反应详情

温度

130 °C

Into a 100-mL 3-necked round-bottom flask, was placed a solution of 6-bromo-1-phenyl-1,2-dihydroindazol-3-one (7 g, 24.22 mmol, 1.00 equiv) in xylene (50 mL) and P2S5 (21.5 g, 96.85 mmol, 4.00 equiv). The resulting solution was stirred for 1 h at 130° C. in an oil bath. The solids were collected by filtration, washed with ethyl acetate (2×50 mL). The organic layer was washed with water (2×50 mL). The resulting mixture was dried over anhydrous sodium sulfate and concentrated under vacuum to yield 6-bromo-1-phenyl-1H-indazole-3-thiol as a brown solid. MS: 304 (MH+).

1. customInto a 100-mL 3-necked round-bottom flask, was placed
2. filtrationThe solids were collected by filtration
3. washwashed with ethyl acetate (2×50 mL)
4. washThe organic layer was washed with water (2×50 mL)
5. dry with materialThe resulting mixture was dried over anhydrous sodium sulfate
6. concentrationconcentrated under vacuum