反应详情

A solution of 1-(4-chloromethylbenzoyl)-4-(2-naphthalenesulfonyl)piperazine (300 mg), potassium carbonate (200 mg) and diisopropylamine (4 ml) in DMF (6 ml) was stirred at 100° C. for 10 hours and concentrated. To the residue was added ethyl acetate, and the mixture was washed with water, and extracted with 1 N hydrochloric acid. The extract was made alkaline with sodium hydroxide solution and extracted with dichloromethane. The extract was dried and concentrated. The residue was purified with silica gel column chromatography (hexane:ethyl acetate=1:2) to give the title compound (70 mg).

1. concentrationconcentrated
2. additionTo the residue was added ethyl acetate
3. washthe mixture was washed with water
4. extractionextracted with 1 N hydrochloric acid
5. extractionextracted with dichloromethane
6. customThe extract was dried
7. concentrationconcentrated
8. customThe residue was purified with silica gel column chromatography (hexane:ethyl acetate=1:2)