反应 #1365725

ord-0fbb8ea3211e486a94fd03207182a651

反应方程式

COC(=O)c1cc(N)c(F)cc1Cl
2-fluoro-4-chloro-5-methoxycarbonylaniline
O=C(Cl)OC(Cl)(Cl)Cl
diphosgene
COC(=O)c1cc(N=C=O)c(F)cc1Cl
2-fluoro-4-chloro-5-methoxycarbonylphenyl isocyanate
收率 95.8%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGThe reaction mixture was stirred at room temperature for one hour
  2. 2
    温度heated
  3. 3
    温度to reflux for 4 hours
  4. 4
    温度The mixture was then cooled to room temperature
  5. 5
    其他the solvents were evaporated under reduced pressure

实验过程

A solution of 2-fluoro-4-chloro-5-methoxycarbonylaniline (1.0 g, 5 mmol) in THF (10 mL) was added dropwist to a solution of diphosgene (2.0 g, 10 mmol) in toluene (20 mL) with stirring at room temperature. The reaction mixture was stirred at room temperature for one hour and then heated to reflux for 4 hours. The mixture was then cooled to room temperature and the solvents were evaporated under reduced pressure to give 1.1 g of 2-fluoro-4-chloro-5-methoxycarbonylphenyl isocyanate as a solid. This was used for the next step without further purification.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06444615B1uspto-grants-2002_09