HRID2088406

反应详情

EQUATION

反应方程式

HRID 2088406 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

100 mg (0.38 mmol) of [3-(5-bromopyrimidin-2-yl)phenyl]methanol and 51 μl (0.56 mmol) of methyl acrylate are suspended in 2 ml of DMF, and 20 mg (0.075 mmol) of triphenylphosphine, 222 mg (2.26 mmol) of potassium acetate and 157 mg (0.57 mmol) of tetra-n-butylammonium chloride are added. The reaction mixture is degassed, flushed with argon, and 17 mg (0.075 mmol) of palladium(II) acetate are added under an argon atmosphere. The mixture is heated at 80° C. for 2 h. After cooling, water is added, during which a pale-grey precipitate forms. This is filtered off with suction, washed with water and dried in vacuo. The product is reacted further without further purification; yield: 111 mg; HPLC: Rt.=2.42 min (method A); LC-MS: 271 (M+H).

WORKUP

后处理

  1. customThe reaction mixture is degassed
  2. additionare added under an argon atmosphere
  3. temperatureAfter cooling
  4. filtrationThis is filtered off with suction
  5. washwashed with water
  6. customdried in vacuo
  7. customThe product is reacted further without further purification
  8. custom=2.42 min (method A)