HRID1669734

反应详情

EQUATION

反应方程式

HRID 1669734 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 4-bromo-1-naphthalenecarboxylic acid (9.42 g), triethylamine (25 ml), palladium acetate (0.85 g), triphenylphosphine (0.98 g) and methyl acrylate (9.68 g) in anhydrous DMF (95 ml) was heated to 100° C. for 1 h under nitrogen. The mixture was allowed to cool to room temperature, filtered through Celite and washed with diethyl ether/water. The filtrate was extracted with ether, then with EtOAc. The aqueous phase was acidified to approximately pH 1 with 2 M aqueous hydrogen chloride. The solid was filtered, washed with water and dried at 40° C. under vacuum, to afford the title compound (8.2 g).

WORKUP

后处理

  1. temperatureto cool to room temperature
  2. filtrationfiltered through Celite
  3. washwashed with diethyl ether/water
  4. extractionThe filtrate was extracted with ether
  5. filtrationThe solid was filtered
  6. washwashed with water
  7. customdried at 40° C. under vacuum