HRID63909
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
PROCEDURE
实验过程
To a solution of 2-(3-(3-ethoxy-3-oxopropyl)ureido)-4-methylthiophene-3-carboxylate (470 mg, 1.5 mmol) in EtOH (10 mL) was added sodium ethoxide (203 mg, 2.19 mmol, freshly prepared). The reaction was heated at reflux for 4 h, concentrated, acidified with 1N HCl until PH=1 then extracted with EA (2×10 mL). The combined organic layers were dried over Na2SO4 and concentrated to give ethyl 3-(5-methyl-2,4-dioxo-1,2-dihydrothieno[2,3-d]pyrimidin-3(4H)-yl)propanoate (330 mg, 82% yield) as a yellow thick oil. LCMS: MH+ 255 and TR=0.718 min. Used without further purification.
WORKUP
后处理
- customfreshly prepared)
- temperatureThe reaction was heated
- temperatureat reflux for 4 h
- concentrationconcentrated
- extractionthen extracted with EA (2×10 mL)
- dry with materialThe combined organic layers were dried over Na2SO4
- concentrationconcentrated