反应 #1365724

ord-eaa96b30c2e14c0296c337f5edba84f2

反应方程式

Nc1cc(OC2CCCC2)c(Cl)cc1F
2-fluoro-4-chloro-5-cyclopentyloxyaniline
O=C(Cl)C(=O)Cl
oxalyl chloride
Cl
HCl
O=C=Nc1cc(OC2CCCC2)c(Cl)cc1F
2-fluoro-4-chloro-5-cylcopentyloxyphenyl isocyanate
收率 86.0%

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 1 hour
  2. 2
    温度heated
  3. 3
    其他the solvents were removed at reduced pressure

实验过程

A solution of 2-fluoro-4-chloro-5-cyclopentyloxyaniline (1.0 g, 5 mmol) in toluene (50 mL) was added dropwise to a solution of oxalyl chloride (2.0 g, 10 mmol) in toluene (20 mL) with stirring. The reaction mixture was stirred at room temperature for 1 hour and then heated to reflux for 4 hours until HCl evolution ceased. The mixture was cooled down to room temperature and the solvents were removed at reduced pressure to give 1.1 g of 2-fluoro-4-chloro-5-cylcopentyloxyphenyl isocyanate as an oily product. This was used in the next step without further purification.

来源

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