反应详情

2.4 g of 1,3-dimethyl-4-[(2-nitrophenyl)amino]pyrazole-5-carboxylic acid phenyl ester are hydrogenated in 150 ml of toluene and 5 ml of glacial acetic acid using 0.75 g of 10% strength palladium-on-charcoal at room temperature for 2.1 hours in a circulatory hydrogenation apparatus. The solution is filtered and concentrated in vacuo; the residue is chromatographed over a silica gel column using 1:1 petroleum ether (50°/70° C.)/ethyl acetate to yield 1.1 g of 1,3-dimethyl-1,4,9,10-tetrahydropyrazolo[4,3-b][1,5]benzodiazepin-10-one, mp 189° to 190° C.

1. filtrationThe solution is filtered
2. concentrationconcentrated in vacuo
3. customthe residue is chromatographed over a silica gel column
4. custom1:1 petroleum ether (50°/70° C.)/ethyl acetate