反应详情

A solution of crude 8,9-dihydro-10-methyl-7-[(5-methyl-1-trityl-1H-imidazol-4-yl)methyl]-pyrido[1,2-a]indol-6(7H)-one in acetic acid (50 ml) and water (15 ml) was stirred at 45° C. for 2 hours and then at 65° C. for 2 hours. After evaporation of the solvent, the residue was diluted with water, neutralized with an aqueous sodium bicarbonate solution, and extracted three times with methylene chloride. The organic layer combined was washed with water and brine, dried over anhydrous magnesium sulfate, and evaporated in vacuo. Purification of the residue with silica gel column chromatography (10% methanol-methylene chloride) gave 8,9-dihydro-10-methyl-7-[(5-methyl-1H-imidazol-4-yl)methyl]pyrido[1,2-a]indol-6(7H)-one (1.0 g) as crystals.

1. customAfter evaporation of the solvent
2. additionthe residue was diluted with water
3. extractionextracted three times with methylene chloride
4. washThe organic layer combined was washed with water and brine
5. dry with materialdried over anhydrous magnesium sulfate
6. customevaporated in vacuo
7. customPurification of the residue with silica gel column chromatography (10% methanol-methylene chloride)