反应 #1350581

ord-b11a3db627c248289e05d0460f005f70

反应方程式

Cc1c(C#N)ccc(S)c1C#N
3-methyl-2,4-dicyanothiophenol
[Na+].[OH-]
NaOH
COS(=O)(=O)OC
dimethyl sulfate
CSc1ccc(C#N)c(C)c1C#N
3-Methyl-2,4-dicyanothioanisole

溶剂

反应条件

温度
25°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONwere then added dropwise at 25-35° C
  2. 2
    其他after which a solid had precipitated out
  3. 3
    过滤which was filtered off with suction
  4. 4
    洗涤washed twice with water
  5. 5
    其他recrystallized from glacial acetic acid/water

实验过程

50 g (0.29 mol) of 3-methyl-2,4-dicyanothiophenol were added to a solution of 23 g (0.58 mol) of NaOH in 400 ml of water, and 73 g (0.58 mol) of dimethyl sulfate were then added dropwise at 25-35° C. The mixture was stirred at 25° C. for 16 h, after which a solid had precipitated out, which was filtered off with suction, washed twice with water and then recrystallized from glacial acetic acid/water. Yield: 43 g (80%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06541423B1uspto-grants-2003_04