HRID1689927

反应详情

EQUATION

反应方程式

HRID 1689927 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-(3-Methoxy-benzoylamino)-thiophene-2-carboxylic acid methyl ester, 24, (12.78 g) was added to methanol (200 mL) previously saturated with ammonia. The mixture was placed in a bomb reactor, and heated to 100° for 2 days. The solvent was then removed in vacuo and the resulting residue was suspended in isopropanol (250 mL); 2M sodium hydroxide solution was then added (83 mL), and the mixture was heated to reflux for 5 hours. The reaction mixture was then cooled and acidified to pH 1. 2-(3-methoxy-phenyl)-3H-thieno[3,2-d]pyrimidin-4-one, 25, (12.16 g) was collected as a white solid.

WORKUP

后处理

  1. customThe mixture was placed in a bomb reactor
  2. temperatureheated to 100° for 2 days
  3. customThe solvent was then removed in vacuo
  4. addition2M sodium hydroxide solution was then added (83 mL)
  5. temperaturethe mixture was heated
  6. temperatureto reflux for 5 hours
  7. temperatureThe reaction mixture was then cooled
  8. custom2-(3-methoxy-phenyl)-3H-thieno[3,2-d]pyrimidin-4-one, 25, (12.16 g) was collected as a white solid