反应详情

N-methylpiperazine 3.6 mL, N,N-diisopropylethylamine 5.7 mL and tetrahydrofuran 31 mL were mixed and dropped into a solution of 4-chloro-3-nitrobenzenesulfonyl chloride 8.19 g in tetrahydrofuran 51 mL, under cooling with ice, followed by stirring for 30 minutes under cooling with ice. The stirring was then continued for 17 hours at room temperature. The solvent was distilled off and the residue was poured in water, of which pH was raised to 9 with saturated aqueous sodium hydrogencarbonate solution, followed by extraction with ethyl acetate-tetrahydrofuran mixed solvent. The organic layer was washed with saturated brine, dried over magnesium sulfate, and from which the solvent was distilled off. Recrystallizing the crude product from ethyl acetate-hexane mixed solvent, 4.29 g of the title compound was obtained.

1. temperatureunder cooling with ice
2. temperatureunder cooling with ice
3. waitThe stirring was then continued for 17 hours at room temperature
4. distillationThe solvent was distilled off
5. additionthe residue was poured in water, of which pH
6. temperaturewas raised to 9 with saturated aqueous sodium hydrogencarbonate solution
7. extractionfollowed by extraction with ethyl acetate-tetrahydrofuran mixed solvent
8. washThe organic layer was washed with saturated brine
9. dry with materialdried over magnesium sulfate
10. distillationfrom which the solvent was distilled off
11. customRecrystallizing the crude product from ethyl acetate-hexane mixed solvent