HRID1699746

反应详情

EQUATION

反应方程式

HRID 1699746 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 3-(6,7-dibromo-2,3-dihydrobenzofuran-5-yl)propionic acid (10.0 g, 28.6 mmols), dichloromethane (35 mL), thionyl chloride (5.11 g, 40.8 mmols) and N,N-dimethylformamide (30 mg) was heated to reflux for 1 hour. After cooling, aluminum chloride (4.66 g, 43.3 mmols) was added to the reaction mixture a trot more than 0° C. and then the mixture was stirred for 30 min. The reaction mixture was poured into precooled methanol (200 mL), then stirred for 30 min. Crystals precipitated were collected by filtration, washed with water (500 mL) followed by methanol (500 mL) to obtain 7.9 g (yield: 89%) of the title compound.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 1 hour
  3. temperatureAfter cooling
  4. stirringstirred for 30 min
  5. customCrystals precipitated
  6. filtrationwere collected by filtration
  7. washwashed with water (500 mL)