??Preparation of 2-(trifluoromethoxy)aniline hydrochloride:
In a 1000mL four-necked flask, 200g (1.92 mol) hydrochloric acid, 100g (0.565 mol) o-amino (trifluoromethoxy)benzene and 80g of water were added sequentially at room temperature with stirring for 1h, and the temperature of the reaction was controlled to be in the range of 0-30??, and 380g of salt-forming reaction solution containing 2-(trifluoromethoxy)aniline hydrochloride was obtained. Salt-forming reaction solution containing 2-(trifluoromethoxy)aniline hydrochloride was obtained.
??Preparation of 2-(trifluoromethoxy)benzene diazonium salt:
In the stirring state, 120g (0.579 mol) of sodium nitrite aqueous solution was added dropwise to 380g of the salting reaction solution obtained in step ??, and the temperature of the reaction was controlled to be from -20 to 5 ??, and the addition of the dropwise solution was completed in 1 h. The reaction solution was kept warm for 1 h, and 500g of the diazonium reaction solution containing the diazonium salt of 2-(trifluoromethoxy)benzene was obtained. reaction solution.
?? Preparation of 2-(trifluoromethoxy)benzenesulfonyl chloride:
In a 2000mL four-necked flask, 400g (3.84mol) hydrochloric acid, 10g (0.0587mol) were added sequentially.
copper chloride and 80.0 g (0.769 mol) sodium bisulfite as substrate, and under stirring condition, 500 g of the obtained from step ?? was added to the reaction solution.
to the diazotization reaction solution at -20 ~ 5 ??, added dropwise to the substrate, 5h dropwise finished, holding 1h, static partition
Layer, split the oil layer, add 400g of water, stirring 0.5h, static layering 0.5h, split the oil layer, to get 142g (content 88%) 2-(trifluoromethoxy)benzenesulfonyl chloride, yield 84.9%.