反应详情

A mixture of 13.0 g of 4-(2,4-dichlorobenzoyl)-N-acetyl-piperidine, 6.8 g of hydroxylamine hydrochloride, 13.5 g of ammonium acetate, 127 ml of ethanol and 43 ml of water was stirred and heated at 130° for 24 hrs. The reaction mixture was evaporated and 1.3 l of water was added to the residue. The water was decanted from the oil and the oil was dissolved in about 150 ml dichloromethane. After washing with about 150 ml of water, drying over anhydrous magnesium sulfate and evaporating the solvent, an oil was obtained, which after crystallization from methanol/ether gave 4.25 g (31.1%) of product, mp, 167°-168°.

1. temperatureheated at 130° for 24 hrs
2. customThe reaction mixture was evaporated
3. addition1.3 l of water was added to the residue
4. customThe water was decanted from the oil
5. dissolutionthe oil was dissolved in about 150 ml dichloromethane
6. washAfter washing with about 150 ml of water
7. dry with materialdrying over anhydrous magnesium sulfate
8. customevaporating the solvent
9. customan oil was obtained
10. customwhich after crystallization from methanol/ether