反应 #569866

ord-f8c2a018224849f9bbfb6a397fc53d32

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度under reflux
  2. 2
    其他The organic phase was separated off
  3. 3
    干燥dried over potassium carbonate
  4. 4
    其他evaporated down
  5. 5
    其他the residue was recrystallised from hexane/diethyl ether

实验过程

3.5 ml of 30% strength perhydrol were added to a mixture of 6.5 g (0.025 mol) of 2-[2-(2,3-dimethylphenyl)-hydrazino]-2-thiazoline hydrochloride, 60 ml of methylene chloride and 50 ml of 2N sodium hydroxide solution. The mixture was stirred for 18 hours under reflux, and a further 2 ml of perhydrol were added after 6 hours, and another 1 ml of perhydrol after 12 hours. The organic phase was separated off, dried over potassium carbonate and evaporated down, and the residue was recrystallised from hexane/diethyl ether. Mp. 74° to 79°, yield 4.1 g (74% of theory).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04575501uspto-grants-1986_03