反应详情

温度

25 °C

N-(6-Bromo-7-oxo-4,5,6,7-tetrahydro-benzothiazol-2-yl)-acetamide (Stage T.3, 473 mg, 1.635 mmol) was dissolved in MeOH (10 mL), 2,2-dimethylthio propionamide (230 mg, 1.962 mmol) and ammonium phosphomolybdate (307 mg, 0.164 mmol) were added, and the RM was stirred at 25° C. for 20 h. The RM was then stood for 2 days before stirring at 50° C. for 24 h. The mixture was extracted with EtOAc/H2O. The organic layers were dried over Na2SO4 and evaporated. The crude material was chromatographed with 30 g of silica gel, eluent DCM/MeOH=99:1. Fractions containing the product were evaporated and lyophilized from dioxane to give 225 mg of the title compound as a white solid (M+H=308; M−H=306; tR 5.525 min (Method F)).

1. waitThe RM was then stood for 2 days
2. stirringbefore stirring at 50° C. for 24 h
3. extractionThe mixture was extracted with EtOAc/H2O
4. dry with materialThe organic layers were dried over Na2SO4
5. customevaporated
6. customThe crude material was chromatographed with 30 g of silica gel, eluent DCM/MeOH=99:1
7. additionFractions containing the product
8. customwere evaporated