HRID60343
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 140 °C
PROCEDURE
实验过程
To a solution of (E)-3-(3-methyl-5-nitro-2,6-dioxo-4-(3-(trifluoromethoxy)styryl)-2,3-dihydro pyrimidin-1(6H)-yl)propyl acetate (50 mg, 0.109 mmol) in HCOOH (3 mL) was added Na2S2O4 (114.0 mg, 0.655 mmol). The reaction was heated at 140° C. for 5 h, cooled to RT then diluted with EA (20 mL) and water (20 mL). The organic layer was dried over Na2SO4 and concentrated to give 3-(1-methyl-2,4-dioxo-6-(3-(trifluoromethoxy)phenyl)-1H-pyrrolo[3,2-d]pyrimidin-3(2H,4H,5H)-yl)propyl acetate (20 mg, 43.1% yield) as an oil. LCMS: MH+ 426 and TR=1.597 min. Used without further purification.
WORKUP
后处理
- temperaturecooled to RT
- dry with materialThe organic layer was dried over Na2SO4
- concentrationconcentrated