HRID1594936

反应详情

EQUATION

反应方程式

HRID 1594936 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A solution of Example 28B (300 mg, 1 mmol), palladium (II) acetate (22 mg, 0.1 mmol) and 1-1′-bis(diphenyphosphino)ferrocene (111 mg, 0.2 mmol) was stirred in DMF (3 mL) for 15 min, treated with Cs2CO3 (813 mg, 2.5 mmol) and 3-methoxyphenylboronic acid (228 mg, 1.5 mmol), stirred for 20 min at 80° C., cooled, treated with pH 7 buffer (10 mL) and extracted with diethyl ether. The ether extracts were dried (MgSO4), concentrated and purified on silica gel with 10% ethyl acetate/haexane to provide 140 mg of the title compound as a white solid.

WORKUP

后处理

  1. temperaturecooled
  2. additiontreated with pH 7 buffer (10 mL)
  3. extractionextracted with diethyl ether
  4. dry with materialThe ether extracts were dried (MgSO4)
  5. concentrationconcentrated
  6. custompurified on silica gel with 10% ethyl acetate/haexane