反应详情

KOtBu (76 mg, 0.68 mmol) was added to a solution of pyrazole (51 mg, 0.76 mmol) in DMSO (1 ml) at 0° C. in a sealed tube and the mixture was stirred at room temperature for 15 min. 1-Chloro-5H-6-thia-4,5-diaza-chrysene 6,6-dioxide 305 (80 mg, 0.252 mmol) was added and the mixture was heated at 100° C. for 4 h. After cooling, the mixture was poured onto ice and the aqueous was extracted with iPA: chloroform (30:70). The organic phase was dried (Na2SO4) and concentrated in vacuo. The crude residue was purified by column chromatography with chloroform/MeOH (98:2) to give the title compound (25 mg, 29%).

1. temperaturethe mixture was heated at 100° C. for 4 h
2. temperatureAfter cooling
3. additionthe mixture was poured onto ice
4. extractionthe aqueous was extracted with iPA
5. dry with materialThe organic phase was dried (Na2SO4)
6. concentrationconcentrated in vacuo
7. customThe crude residue was purified by column chromatography with chloroform/MeOH (98:2)