Hydrochloric Acid → Benzene, 2-chloro-1,3-difluoro-

Temperature

60 °C

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).

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

ORD record

ord-e7249afac69a42629cb56bae8666883e

Source dataset

uspto-grants-2010_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07758931B2