反应详情

Nine grams (0.033 mol) of 5-chlorocarbonyl-5,10-dihydro-11H-dibenzo[b,e][1,4]diazepin-11-one, 5.3 gm (0.05 mol) of sodium carbonate, and 5.2 gm (0.036 mol) of 1-methyl-4-methylamino-piperidine were refluxed in 150 ml of acetonitrile for 15 minutes under stirring. The mixture was filtered while hot, and then the filtrate was placed on a silica gel column and eluted first with acetonitrile and then with a methylene chloride/ethyl acetate/cyclohexane/methanol/ammonia (175:75:23:23:3) mixture. The desired fraction was concentrated by evaporation in vacuo, and the residue was recrystallized from acetonitrile.

1. filtrationThe mixture was filtered while hot, and then the filtrate
2. washeluted first with acetonitrile
3. concentrationThe desired fraction was concentrated by evaporation in vacuo
4. customthe residue was recrystallized from acetonitrile