HRID2233777

反应详情

EQUATION

反应方程式

HRID 2233777 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 104 mg portion of palladium acetate and 5 ml of TEA were added one by one to 50 ml of acetonitrile solution containing 7.44 g of 3-iodobenzoic acid and 3.9 ml of ethyl acrylate, and the mixture was sealed in a tube and heated at 100° C. for about 12 hours. After spontaneous cooling, the catalyst was removed by filtration while washing with appropriate amounts of methanol and ethyl acetate, and the filtrate was evaporated under a reduced pressure. The thus formed crude crystals were recrystallized from a small amount of ethanol to obtain 5.82 g (88%) of 3-(3-ethoxy-3-oxoprop-1-en-1-yl)benzoic acid as white crystals. FA: 221

WORKUP

后处理

  1. customthe mixture was sealed in a tube
  2. customAfter spontaneous cooling, the catalyst was removed by filtration
  3. washwhile washing with appropriate amounts of methanol and ethyl acetate
  4. customthe filtrate was evaporated under a reduced pressure
  5. customThe thus formed crude crystals
  6. customwere recrystallized from a small amount of ethanol