反应详情

温度

150 °C

A mixture of methyl 4-(1,4-dihydroindeno[1,2-c]pyrazol-3-yl)benzoate (100 mg) and N-(2-aminoethyl)morpholine (0.5 ml) was stirred and heated at 150° C. for 5 hours. The mixture was cooled and washed with petroleum ether, b.p. 40-60° C. (20 ml). The mixture was dissolved in a mixture of dichloromethane/IMS/triethyl-amine (25:2:1) and purified by flash column chromatography on silica using the same solvent mixture as the mobile phase. Appropriate fractions were collected, combined and evaporated to give a gum which was dissolved in dichloromethane, washed with water, then dried, filtered and evaporated to give a solid which was triturated with ether and filtered to give N-(2-morpholinoethyl)-4-(1,4-dihydroindeno[1,2-c]pyrazol-3-yl)benzamide monohydrate, m.p. 210-214° C.

1. temperatureThe mixture was cooled
2. washwashed with petroleum ether, b.p. 40-60° C. (20 ml)
3. dissolutionThe mixture was dissolved in a mixture of dichloromethane/IMS/triethyl-amine (25:2:1)
4. custompurified by flash column chromatography on silica using the same solvent mixture as the mobile phase
5. customAppropriate fractions were collected
6. customevaporated
7. customto give a gum which
8. washwashed with water
9. customdried
10. filtrationfiltered
11. customevaporated
12. customto give a solid which
13. customwas triturated with ether
14. filtrationfiltered