HRID1723690

反应详情

EQUATION

反应方程式

HRID 1723690 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

5

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

Pd(PPh3)4 (0.313 g, 0.271 mmol) and trans-2-phenylvinylboronic acid (1.105 g, 7.468 mmol) were added to a mixture of 6-bromo-2-(2-chlorophenylamino)-3,4-difluorobenzoic acid methyl ester (2.00 g, 5.31 mmol) in 35 mL DME and 8 mL 2.0 M aqueous K2CO3 solution. The reaction mixture was heated under a N2 atmosphere to 90° C. and stirred for 16 hours. After cooling to room temperature, the reaction mixture was diluted with ethyl acetate and water and the layers separated. The organic layer was dried (MgSO4) and concentrated under reduced pressure. Purification by flash column chromatography gave 1.20 g (56%) clean desired product.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. customthe layers separated
  3. dry with materialThe organic layer was dried (MgSO4)
  4. concentrationconcentrated under reduced pressure
  5. customPurification by flash column chromatography