HRID1429157

反应详情

EQUATION

反应方程式

HRID 1429157 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

Compound 10f (43 mg, 72.4 mmol), phenylboronic acid (13 mg, 109 μmol) and (PPh3)2PdCl2 (5 mg, 7.2 umol) were mixed in a microwave reaction vial and heated in the microwave at 120° C. for 20 min. The reaction mixture was then quenched by addition of citric acid (20 ml) and extracted 2 times with DCM (10 ml). The combined organic phases were washed with water (2×10 ml) and brine (10 ml), dried over MgSO4 and filtered. The solvent was removed in vacuo and the crude product was purified by preparative LC-MS which gave the title compound (5.9 mg, 13%), (ESI+)=636 (MH+).

WORKUP

后处理

  1. customThe reaction mixture was then quenched by addition of citric acid (20 ml)
  2. extractionextracted 2 times with DCM (10 ml)
  3. washThe combined organic phases were washed with water (2×10 ml) and brine (10 ml)
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customThe solvent was removed in vacuo
  7. customthe crude product was purified by preparative LC-MS which