HRID535384

反应详情

EQUATION

反应方程式

HRID 535384 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of 6-chloro-4-(trifluoromethyl)pyridin-2-amine (1.0 g, 5.09 mmol) ethynylbenzene (779 mg, 7.63 mmol), 1,1′-Bis(diphenylphosphino)ferrocene]dichloro-palladium(II) (372 mg, 0.51 mmol), copper(I) iodide (96 mg, 0.51 mmol), triethylamine (1.8 ml, 12.7 mmol), ACN (10 ml) and THF (5 ml) is stirred for 6 h at 90° C. The mixture is concentrated in vacuo, water is added (100 ml) and the mixture extracted with EtOAc. The combined organic layers are dried over MgSO4 and concentrated in vacuo. The product is purified by NP chromatography. Yield: 680 mg (51%). HPLC-MS: M+H=263.

WORKUP

后处理

  1. concentrationThe mixture is concentrated in vacuo, water
  2. additionis added (100 ml)
  3. extractionthe mixture extracted with EtOAc
  4. dry with materialThe combined organic layers are dried over MgSO4
  5. concentrationconcentrated in vacuo
  6. customThe product is purified by NP chromatography