反应 #74503

ord-541340427c5d4696b208240ea8e76d24

反应条件

温度
70°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度cooled to ambient temperature
  2. 2
    其他The resulting solid was isolated by filtration
  3. 3
    其他dried in vacuo

实验过程

To a solution of 2,4-dichlorobenzoic acid (compound 80, 25.0 g, 131 mmol) in chlorosulfonic acid (100 mL) was added bromine (3.4 mL, 65 mmol) and sulfur (0.20 g, 6.6 mmol). The reaction mixture was stirred at 70° C. overnight and then cooled to ambient temperature. The reaction mixture was poured into iced water. The resulting solid was isolated by filtration and dried in vacuo to yield title compound (32.9 g, 93%) as pale brown solid.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08541380B2uspto-grants-2013_09