反应详情

温度

75 °C

A mixture of 7-[(1-benzyl-5-methyl-1H-imidazol-4-yl)methyl]-10-[(dimethylamino)methyl]-8,9-dihydropyrido-[1,2-a]indol-6(7H)-one (215 mg), ammonium formate (318 mg), 10% palladium on carbon (107 mg), water (1 ml), ethanol (2 ml), and tetrahydrofuran (1 ml) was heated at 75° C. for 40 minutes and then cooled. Ammonium formate (300 mg), 10% palladium on carbon (110 mg), water (1 ml), and ethanol (2 ml) were added successively to the reaction mixture. Heating at 75° C. was continued for further 1 hour 20 minutes. After cooling, the reaction mixture was filtered and the residue was washed with 10% methanol-chloroform. The filtrate was evaporated in vacuo. The residue was diluted with water and extracted three times with 10% methanol-chloroform. The organic layer was washed with water and brine, dried over anhydrous magnesium sulfte, and evaporated in vacuo. Silica gel column chromatography of the residue using 5% methanol-chloroform as eluent gave 8,9-dihydro-10-methyl-7-[(5-methyl-1H-imidazol-4-yl)methyl]pyrido[1,2-a]indol-6(7H)-one (108 mg).

1. temperaturecooled
2. temperatureHeating at 75° C.
3. temperatureAfter cooling
4. filtrationthe reaction mixture was filtered
5. washthe residue was washed with 10% methanol-chloroform
6. customThe filtrate was evaporated in vacuo
7. additionThe residue was diluted with water
8. extractionextracted three times with 10% methanol-chloroform
9. washThe organic layer was washed with water and brine
10. dry with materialdried over anhydrous magnesium sulfte
11. customevaporated in vacuo