Hydrochloric Acid → N-(2-Hydroxyethyl)-4-methoxy-N,2,6-trimethylbenzenesulfonamide

Beteiligte Stoffe

Reaktionsbedingungen

Reaktionsschritte

10.00 kg (73.42 mol) of 3,5-dimethylanisol (A) were dissolved in 35.0 L of dichloromethane. After cooling to −15±5° C. a solution of 17.46 kg (149.86 mol) of chlorosulphonic acid in 20.0 L dichloromethane was metered in and the mixture was stirred for approx. another 30 minutes at −15±5° C. Then the reaction mixture was metered into a solution of 15.0 kg sodium chloride in 85.0 L of water that had been cooled to −7±5° C., and diluted with 15.0 L of dichloromethane. The organic phase was separated off, diluted with 15.0 L of dichloromethane and washed with 30.0 L of sodium hydrogen carbonate solution (5%). After separation of the organic phase once again and dilution with 10 L of dichloromethane, a solution of 11.58 kg (154.20 mol) N-methylaminoethanol in 10.0 L of dichloromethane was slowly metered in at 10±5° C. After the reaction had ended 45.0 L of HCl (3%) and 5.0 L of water were added. The organic phase was separated off, diluted with 10.0 L dichloromethane and the solvent was totally eliminated from the product (C) in vacuo.

Herkunft & Nachweise