反应详情

To a solution of 1-(6-chloronaphthalene-2-sulfonyl)piperazine hydrochloride(100 mg), 4-diisopropylaminomethyl-2-methoxybenzoic acid (77 mg), triethylamine (35 mg) and HOBt (43 mg) in DMF (10 ml) was added WSC hydrochloride (61 mg) under ice-cooling, and the solution was stirred at room temperature for 4 hours and concentrated. To the residue were added ethyl acetate and sodium bicarbonate solution. The organic layer was separated, 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 and the residue was crystallized with ether to give colorless crystals of the title compound (99 mg).

1. temperaturecooling
2. concentrationconcentrated
3. additionTo the residue were added ethyl acetate and sodium bicarbonate solution
4. customThe organic layer was separated
5. washwashed with water
6. extractionextracted with 1 N hydrochloric acid
7. extractionextracted with dichloromethane
8. customThe extract was dried
9. concentrationconcentrated
10. customthe residue was crystallized with ether