HRID257361

反应详情

EQUATION

反应方程式

HRID 257361 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 13.75 g (0.0967 mole) of 2-fluoro-4-methoxyaniline in 120 mL of toluene was slowly added over a period of 30 minutes a solution of 19.13 g (0.0967 mole) of trichloromethyl chloroformate in 30 mL of toluene. During the addition the temperature rose to 35° C. The reaction mixture was stirred without external heating for 30 minutes and then heated at reflux for approximately 17 hours. At the end of this time all of the solvent was removed by distillation, leaving 2-fluoro-4-methoxyphenyl isocyanate as a purple liquid, which was used immediately in Step D.

WORKUP

后处理

  1. additionDuring the addition the temperature
  2. customrose to 35° C
  3. temperaturewithout external heating for 30 minutes
  4. temperatureheated
  5. temperatureat reflux for approximately 17 hours
  6. customAt the end of this time all of the solvent was removed by distillation