反应详情

Batch size: 38.0 g (<89.5 mmol) 2-[4-(1-phenyl-1,2,4,5-tetrahydro-benzo[d]azepin-3-yl)-butyl]-isoindol-1,3-dione and 8.7 ml (179 mmol) hydrazine hydrate in 200 ml ethanol. The reaction mixture is filtered and the filtrate is concentrated under vacuum. The residue is taken up in 400 ml dichloromethane and washed twice each with 50 ml 10% NaCH solution. The organic phase is dried over sodium sulfate and, subsequently, the solvent is removed under vacuum. The purification occurs chromatographically over silica gel with CHCl3/CH3OH/TEA (95/5/0 to 90/9/1): Yield 15.6 g (59%).

1. filtrationThe reaction mixture is filtered
2. concentrationthe filtrate is concentrated under vacuum
3. washwashed twice each with 50 ml 10% NaCH solution
4. dry with materialThe organic phase is dried over sodium sulfate
5. customsubsequently, the solvent is removed under vacuum
6. customThe purification