HRID1521565

反应详情

EQUATION

反应方程式

HRID 1521565 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a stirred solution of 3,5-dibromo-4-chloropyridine (X, 0.5 g, 1.84 mmol) and cyclopropylboronic acid (0.17 g, 2.02 mmol), cesium carbonate (1.19 g, 3.68 mmol) in the mixture of 1,4-dioxan (10 mL) and water (2 mL). The reaction mass was purged with nitrogen for 15 min. Then catalyst Pd (dppf)2Cl2 (0.075 g, 0.09 mmol) was added and allowed to stir at 100° C. for 4 h. The reaction mixture was filtered through Mite bed and filter bed was thoroughly washed with ethyl acetate. The collected organic parts were concentrated under vacuum to afford the crude compound, which was purified by column chromatography using 10-40% ethyl acetate/hexane as an eluent to obtain title compound. MS (M+1): 233.0.

WORKUP

后处理

  1. customThe reaction mass was purged with nitrogen for 15 min
  2. filtrationThe reaction mixture was filtered through Mite bed
  3. filtrationfilter bed
  4. washwas thoroughly washed with ethyl acetate
  5. concentrationThe collected organic parts were concentrated under vacuum
  6. customto afford the crude compound, which
  7. customwas purified by column chromatography