HRID1892476

反应详情

EQUATION

反应方程式

HRID 1892476 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a solution of 2-fluoro-4-methylbenzoic acid (1.029 g, 6.678 mmol) in carbon tetrachloride (10 ml) were added N-bromosuccinimide (1.189 g, 6.682 mmol) and 2,2′-azobisisobutyronitrile (43.9 mg, 0.267 mmol). After stirring at 90° C. for 30 min and at 100° C. for 2.5 hr, the mixture was cooled to 0° C. The precipitate was collected by filtration and washed with hexane and water to give a crude product. The crude product was dissolved in ethyl acetate (5 ml), and hexane (10 ml) was added. The precipitated solid was collected by filtration, and dried under reduced pressure to give 4-(bromomethyl)-2-fluorobenzoic acid (838.6 mg, 3.599 mmol, yield 53.9%) as a slightly yellow solid.

WORKUP

后处理

  1. temperaturethe mixture was cooled to 0° C
  2. filtrationThe precipitate was collected by filtration
  3. washwashed with hexane and water
  4. customto give a crude product
  5. filtrationThe precipitated solid was collected by filtration
  6. customdried under reduced pressure