HRID1716530

反应详情

EQUATION

反应方程式

HRID 1716530 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A suspension of (6-bromopyridin-2-yl)-(4-methylpyridin-2-yl)amine (1.00 g, 3.79 mmol), 5-acetylthiophene-2-boronic acid (644 mg, 3.79 mmol), tetrakis triphenylphosphine palladium (440 mg, 0.38 mmol), sodium hydrogen carbonate (480 mg, 5.68 mmol) in dimethoxyethane-water (12 ml) was heated and stirred in an Ar stream at 130° C. for 12 hours. Water was added to the reaction solution and extracted with ethyl acetate. After the organic layer was washed with a saturated brine and dried over anhydrous magnesium sulfate, the residue obtained by concentration in vacuo was washed with tetrahydrofuran-ethyl acetate (1:1), dried, and the title compound (426 mg, 36%) was obtained.

WORKUP

后处理

  1. temperaturewas heated
  2. extractionextracted with ethyl acetate
  3. washAfter the organic layer was washed with a saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customthe residue obtained by concentration in vacuo
  6. washwas washed with tetrahydrofuran-ethyl acetate (1:1)
  7. customdried