反应详情

温度

150 °C

A mixture of methyl 4-(1,4-dihydroindeno[1,2-c]pyrazol-3-yl)benzoate (0.3 g) and N,N-diethylethylenediamine (1 ml) was heated at 150° C. for 3.5 hours and then at 180° C. for 2 hours. The mixture was cooled and dissolved in industrial methylated spirit and this solution was preabsorbed onto silica which was applied to the top of a flash column. The column was eluted with dichloromethane/industrial methylated spirit/triethylamine (25:2:1) to give a solid which was stirred with water for 1 hour, filtered and dried under vacuum at 60° C. to give N-(2-diethylaminoethyl)-4-(1,4-dihydroindeno[1,2-c]pyrazol-3-yl)benzamide, m.p. 172-174° C.

1. temperatureThe mixture was cooled
2. customthis solution was preabsorbed onto silica which
3. washThe column was eluted with dichloromethane/industrial methylated spirit/triethylamine (25:2:1)
4. customto give a solid which
5. filtrationfiltered
6. customdried under vacuum at 60° C.