HRID870229

反应详情

EQUATION

反应方程式

HRID 870229 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Into a 100-mL round-bottom flask, was placed a solution of isophthalic acid (10 g, 60.24 mmol, 1.00 equiv) in 98% H2SO4 (60 mL). This was followed by the addition of N-bromosuccinimide (12.80 g, 72.32 mmol, 1.20 equiv), in portions at 60° C. in 10 min. The resulting solution was stirred overnight at 60° C. in an oil bath. The reaction was cooled to room temperature and then quenched by the addition of water/ice. The solids were collected by filtration, and washed with 2×60 mL of hexane. The solid was dried in an oven under reduced pressure. The crude product was purified by re-crystallization from ethyl acetate to give 3 g (20%) of 5-bromoisophthalic acid as a white solid.

WORKUP

后处理

  1. customInto a 100-mL round-bottom flask, was placed
  2. temperatureThe reaction was cooled to room temperature
  3. customquenched by the addition of water/ice
  4. filtrationThe solids were collected by filtration
  5. washwashed with 2×60 mL of hexane
  6. customThe solid was dried in an oven under reduced pressure
  7. customThe crude product was purified by re-crystallization from ethyl acetate