反应详情

A mixture of (2R)-1-[3,5-bis(trifluoromethyl)benzoyl]-4-(4-chloro-2-butynyl)-2-(2-naphthylmethyl)piperazine (300 mg), cis-2,6-dimethylmorpholine (94 mg) and powdered potassium carbonate (210 mg) in dry N,N-dimethylformamide (5 ml) was stirred at room temperature overnight. The reaction mixture was poured into water (50 ml) and extracted with ethyl acetate. The extract was washed with brine and dried over magnesium sulfate. After evaporation of the solvent, the obtained residue was purified by column chromatography on silica gel using a mixture of ethyl acetate and hexane (4:1) as eluent. The obtained product was dissolved in ethyl acetate and treated with 4N hydrogen chloride in ethyl acetate to give (2R)-1-[3,5-bis (trifluoromethyl)benzoyl]-4-[4-(cis-2,6-dimethylmorpholino)-2-butynyl]-2-(2-naphthylmethyl)piperazine dihydrochloride (170 mg).

1. extractionextracted with ethyl acetate
2. washThe extract was washed with brine
3. dry with materialdried over magnesium sulfate
4. customAfter evaporation of the solvent
5. customthe obtained residue was purified by column chromatography on silica gel using
6. additiona mixture of ethyl acetate and hexane (4:1) as eluent
7. dissolutionThe obtained product was dissolved in ethyl acetate
8. additiontreated with 4N hydrogen chloride in ethyl acetate