HRID2356155

反应详情

EQUATION

反应方程式

HRID 2356155 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

550 g of hydrochloric acid was added to a reactor having 270 g of water placed therein, and 129 g of 2,6-difluoroaniline (b1) was further added thereto, followed by stirring for 30 minutes at 60° C. Thereafter, the mixture was cooled to −10° C., and 192.5 g of a 37.6% sodium nitrite aqueous solution was added dropwise thereto over 30 minutes in a temperature range of −10 to −5° C., followed by stirring for 30 minutes at −10° C. The resulting reaction mixture was added to another reactor having 122 g of 30% hydrochloric acid and 22 g of cuprous chloride placed therein over 90 minutes in a temperature range of 25 to 30° C., followed by stirring for 30 minutes in that temperature range. A reaction mixture obtained by the reaction was subjected to steam distillation. The resulting organic phase was washed with water in three times and then dried to obtain 124 g of 2-chloro-1,3-difluorobenzene (b2).

WORKUP

后处理

  1. temperatureThereafter, the mixture was cooled to −10° C.
  2. waitover 30 minutes in a temperature range of −10 to −5° C.
  3. stirringby stirring for 30 minutes at −10° C
  4. customThe resulting reaction mixture
  5. additionwas added to another reactor
  6. waitover 90 minutes in a temperature range of 25 to 30° C.
  7. stirringby stirring for 30 minutes in that temperature range
  8. customA reaction mixture obtained by the reaction
  9. distillationwas subjected to steam distillation
  10. washThe resulting organic phase was washed with water in three times
  11. customdried