反应详情

温度

17.5 °C

A mixture of 4-(1,4-dihydroindeno[1,2-c]pyrazol-3-yl)benzoic acid (0.37 g), dichloromethane (20 ml) and oxalyl chloride (0.26 ml) was stirred at 15-20° C. and then dimethylformamide (3 drops) was added. The mixture was stirred at 15-20° C. for 30 minutes and then warmed at 40° C. for 1 hour. The solvent was removed under reduced pressure to give a solid which was dissolved in dichloromethane (20 ml) and then aniline (0.13 ml) and triethylamine (0.38 ml) were added. The mixture was stirred at ambient temperature under nitrogen for 2 hours and then washed with water, dried, filtered and evaporated to give a solid which was purified by flash column chromatography on silica to give 4-(1,4-dihydroindeno[1,2-c]pyrazol-3-yl)benzanilide, m.p. 186-190° C.

1. stirringThe mixture was stirred at 15-20° C. for 30 minutes
2. temperaturewarmed at 40° C. for 1 hour
3. customThe solvent was removed under reduced pressure
4. customto give a solid which
5. stirringThe mixture was stirred at ambient temperature under nitrogen for 2 hours
6. washwashed with water
7. customdried
8. filtrationfiltered
9. customevaporated
10. customto give a solid which
11. customwas purified by flash column chromatography on silica