反应详情

A solution of 2.1 g of 2-chloro-5-(4-nitro-benzoyl)-6,11-dihydro-5H-dibenz[b,e]azepine in 400 ml of ethyl acetate-ethanol (1:1) and 0.25 g of palladium-on-carbon is hydrogenated in a Parr hydrogenator under 38 pounds per square inch of hydrogen. The mixture is filtered through diatomaceous earth and the filtrate concentrated to dryness. The solid (1.94 g) is dissolved in dichloromethane and the solution filtered through a thin pad of hydrous magnesium silicate. The filter pad is washed with dichloromethane and the filtrate concentrated. The residue is crystallized from dichloromethane-hexane to give 1.43 g of crystals, m.p. 211°-214° C.

1. filtrationThe mixture is filtered through diatomaceous earth
2. concentrationthe filtrate concentrated to dryness
3. dissolutionThe solid (1.94 g) is dissolved in dichloromethane
4. filtrationthe solution filtered through a thin pad of hydrous magnesium silicate
5. washThe filter pad is washed with dichloromethane
6. concentrationthe filtrate concentrated
7. customThe residue is crystallized from dichloromethane-hexane