HRID1008660

反应详情

EQUATION

反应方程式

HRID 1008660 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a DMF solution (0.25 mL) of palladium acetate (38.0 mg, 0.17 μmol), compound 1 (0.50 g, 1.71 mmol), tributylamine (0.41 μL, 1.71 mmol), methyl acrylate (0.38 L, 4.27 mmol), and H2O (1.0 mL) were sequentially added. The reaction solution was allowed to react at 160° C. for 10 minutes using microwaves, and the reaction was traced by TLC. Thereby, the loss of compound 1 was confirmed. The palladium powder was removed by Kiriyama filtration, and then the reaction solution was purified by column chromatography (HexH:AcOEt=3:1), and thus compound 7 (0.26 g, 62%) was obtained as a white powder.

WORKUP

后处理

  1. customto react at 160° C. for 10 minutes
  2. customThe palladium powder was removed by Kiriyama filtration
  3. customthe reaction solution was purified by column chromatography (HexH:AcOEt=3:1)