HRID1173836

反应详情

EQUATION

反应方程式

HRID 1173836 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Add 3-(5-bromo-benzo[b]thiophen-2-ylmethyl)-1-cyclohexyl-pyrrolidin-2-one (250 mg, 0.64 mmol), 2-fluoropyridine-4-boronic acid (200 mg, 1 mmol), LiCl (10 eq) and Pd(PPh3)4 (0.05 eq) into a solution of dioxane (10 mL) and 2M Na2CO3 (2 mL) and heat at 80° C. for 1 hour. Pour the reaction mixture into water and extract with ethyl acetate. Dry over sodium sulfate, filter, and concentrate. Purify by silica gel (20-50% ethyl acetate in hexanes) to give the title compound as a pale yellow powder (260 mg, 58%): MS (APCI-pos mode) m/z (rel intensity): 409.2 (M+H, 100%).

WORKUP

后处理

  1. extractionextract with ethyl acetate
  2. dry with materialDry over sodium sulfate
  3. filtrationfilter
  4. concentrationconcentrate
  5. customPurify by silica gel (20-50% ethyl acetate in hexanes)