反应 #1824321

ord-645eeb2ec2e341e4a2eb5c5729da6535

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度under reflux for 18 hours
  2. 2
    其他the crude product is precipitated by addition of water
  3. 3
    其他recrystallization from n-hexane
  4. 4
    workup.ADDITIONwith addition of active charcoal
  5. 5
    其他gives 5.7 g (16% of theory) of product, which

实验过程

24.4 g (0.1 mol) of 1-(2-ethylhexyl)-2-methylbenzimidazole (prepared by heating N-2-ethylhexyl-o-phenylenediamine in acetic acid/hydrochloric acid), 10.9 g (0.1 mol) of o-aminophenol and 9.6 g (0.3 mol) of sulfur in 100 ml of pyridine are heated under reflux for 18 hours. After cooling to room temperature, the crude product is precipitated by addition of water. Multiple recrystallization from n-hexane with addition of active charcoal gives 5.7 g (16% of theory) of product, which according to melting point, EPLC and UV determination is identical to the compound obtained in Example 7.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05961960uspto-grants-1999_10