反应详情

A suspension of 730 mg(1.83 mmol) of (2R*,4S*)-2-(4-chlorobenzyl)-1-(3,5-dimethyl-benzoyl)-N-acetyl-4-piperidinamine in 6N hydrochloric acid is heated at 100° for 16 hours, during which the starting material dissolves. The reaction mixture is basified with 10% strength aqueous sodium carbonate solution and extracted with ethyl acetate. The combined organic phases are dried over sodium sulfate and evaporated to dryness under reduced pressure. The crude title compound is purified by chromatography on silica geI with dichloromethane/methanol/25% strength ammonia solution (90:10:0.1) as mobile phase and is obtained as almost colourless resin. TLC (dichloromethane/methanol/25% strength ammonia solution; 90:10:0.1):Rf =0.26; FD-MS:(M+I)+=357

1. temperatureis heated at 100° for 16 hours, during which the starting material
2. dissolutiondissolves
3. extractionextracted with ethyl acetate
4. dry with materialThe combined organic phases are dried over sodium sulfate
5. customevaporated to dryness under reduced pressure
6. customThe crude title compound is purified by chromatography on silica geI with dichloromethane/methanol/25% strength ammonia solution (90:10:0.1) as mobile phase
7. customis obtained as almost colourless resin