反应 #814024
ord-f9950dc95a94410486aae253107a9552
反应方程式
Phosgene
4-bromo-2-fluorobenzylamine
hydrochloric acid
4-bromo-2-fluorobenzylamine hydrochloride
→
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温度the mixture is then refluxed
- 2其他to remove the gases phosgene and hydrogen chloride
- 3workup.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.