반응 #934685

반응 방정식

8,9-dihydro-7-[(hydroxy)(1-trityl-1H-imidazol-2-yl)methyl]-10-methylpyrido[1,2-a]indol-6(7H)-one

→

8,9-dihydro-7-[(hydroxy)(1H-imidazol-2-yl)-methyl]-10-methylpyrido[1,2-a]indol-6(7H)-one

수율 71.7%

용매

acetic acid

water

반응 조건

후처리

1. 1
   기타After evaporation of the solvent
2. 2
   workup.ADDITIONthe residue was diluted with water
3. 3
   추출extracted three times with chloroform
4. 4
   세척The organic layer was washed with brine
5. 5
   건조dried over anhydrous magnesium sulfate
6. 6
   기타evaporated in vacuo
7. 7
   기타Purification of the residue with silica gel column chromatography (15% methanol-chloroform)
8. 8
   기타followed by recrystallization from methanol

실험 절차

A solution of 8,9-dihydro-7-[(hydroxy)(1-trityl-1H-imidazol-2-yl)methyl]-10-methylpyrido[1,2-a]indol-6(7H)-one (376 mg) in acetic acid (15 ml) and water (5 ml) was stirred at 60° C. for 2.5 hours. After evaporation of the solvent, the residue was diluted with water, neutralized with an aqueous solution of sodium hydrogencarbonate, and extracted three times with chloroform. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, and evaporated in vacuo. Purification of the residue with silica gel column chromatography (15% methanol-chloroform), followed by recrystallization from methanol, gave 8,9-dihydro-7-[(hydroxy)(1H-imidazol-2-yl)-methyl]-10-methylpyrido[1,2-a]indol-6(7H)-one (148 mg).

출처