反应 #814024

ord-f9950dc95a94410486aae253107a9552

反应方程式

O=C(Cl)Cl
Phosgene
NCc1ccc(Br)cc1F
4-bromo-2-fluorobenzylamine
Cl
hydrochloric acid
Cl.NCc1ccc(Br)cc1F
4-bromo-2-fluorobenzylamine hydrochloride
O=C=NCc1ccc(Br)cc1F
4-bromo-2-fluorobenzyl isocyanate
收率 92.1%

溶剂

反应条件

温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度the mixture is then refluxed
  2. 2
    其他to remove the gases phosgene and hydrogen chloride
  3. 3
    workup.DISTILLATIONThe batch is worked up by distillation

实验过程

A solution of 4-bromo-2-fluorobenzylamine (20.4 g, 0.10 mol) in toluene (300 ml) is saturated with gaseous hydrochloric acid at 25° C. The resulting suspension of the 4-bromo-2-fluorobenzylamine hydrochloride is heated at 100° C. Phosgene is passed in at this temperature. Stirring of the solution, which has eventually become clear, is continued at 100° C. for 1 hour, and the mixture is then refluxed to remove the gases phosgene and hydrogen chloride. The batch is worked up by distillation. 21.2 g of 4-bromo-2-fluorobenzyl isocyanate (boiling point 109° C. at 4 mbar) are obtained. Yield: 92.1% of theory.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05710319uspto-grants-1998_01