HRID240603

反应详情

EQUATION

反应方程式

HRID 240603 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Methyl 4-(4-fluoro-2-hydroxyphenylamino)-5-methylthieno[2,3-d]pyrimidine-6-carboxylate (described in V.1) (1.0 g), 1-(methylsulfonyl)pyrrolidin-3-yl methansulfonate and potassium carbonate (664.0 mg) were combined in DMF (15.0 ml) and heated at 60° C. overnight. The temperature was increased at 80° C. and heated for 6 h again. The reaction mixture was allowed to cool overnight. The mixture was portioned between EtOAc and water. The suspension was fitlered, solid washed with EtOAc and air-dried under vacuum.

WORKUP

后处理

  1. temperatureThe temperature was increased at 80° C.
  2. temperatureheated for 6 h again
  3. temperatureto cool overnight
  4. washsolid washed with EtOAc
  5. customair-dried under vacuum