反应详情

温度

26 °C

A 4 m3 reactor was initially charged with 1773 kg of a 13% by weight solution of 4-chlorophenylboronic acid in tetrahydrofuran at 18-22° C. Within 20 minutes, 538 kg of 25% by weight aqueous sodium hydroxide solution and 140 kg of water were metered in with stirring at 22-30° C. After full addition, the reaction solution was stirred at 22-25° C. for 30 minutes. 2.28 kg of triphenylphosphine, 372 g of palladium(II) chloride and 252 kg of molten 1-chloro-2-nitrobenzene were added to the reaction solution. The reaction solution was heated to 66° C. for 18 h. After full reaction of the 4-chlorophenylboronic acid, the reaction solution was cooled to 45° C. and extracted with 794 kg of 10% by weight aqueous hydrochloric acid. After phase separation, a solution of 4-chloro-2′-nitrobiphenyl in tetrahydrofuran was obtained (conversion 99%).

1. additionAfter full addition
2. stirringthe reaction solution was stirred at 22-25° C. for 30 minutes
3. temperatureThe reaction solution was heated to 66° C. for 18 h
4. temperaturethe reaction solution was cooled to 45° C.
5. extractionextracted with 794 kg of 10% by weight aqueous hydrochloric acid
6. customAfter phase separation