HRID63909

反应详情

EQUATION

反应方程式

HRID 63909 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customfreshly prepared)
  2. temperatureThe reaction was heated
  3. temperatureat reflux for 4 h
  4. concentrationconcentrated
  5. extractionthen extracted with EA (2×10 mL)
  6. dry with materialThe combined organic layers were dried over Na2SO4
  7. concentrationconcentrated