反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThereafter, the mixture was cooled to −10° C.
- waitover 30 minutes in a temperature range of −10 to −5° C.
- stirringby stirring for 30 minutes at −10° C
- customThe resulting reaction mixture
- additionwas added to another reactor
- waitover 90 minutes in a temperature range of 25 to 30° C.
- stirringby stirring for 30 minutes in that temperature range
- customA reaction mixture obtained by the reaction
- distillationwas subjected to steam distillation
- washThe resulting organic phase was washed with water in three times
- customdried