preparation of p c 12 h 25 benzenesulfonylchloride str6 to 50 g 0 153 mole of technical p c 12 h 25 c 6 h 4 so 2 h is added 18 25 g 0 119 mole 11 1 ml of phosphorous oxychloride the mixture is stirred magnetically while the flask is heated in an oil bath at 75 u00b0 80 u00b0 c for 1 hr during this period of heating the bulk of gaseous hcl evolves at a manageable rate stirring is continued while the flask is heated at reflux with the oil bath maintained at 105 u00b0 110 u00b0 for 16 hrs the mixture is cooled to room temperature and with the aid of 100 ml of etoac 50 ml of water and 50 g of ice is transferred to a separatory funnel the etoac layer is washed successively with 100 ml portions of ether 5 nahco 3 and water before discarding each aqueous extract is shaken in another separatory funnel with 50 ml of etoac emulsions are broken by adding 5 ml portions of saturated salt solution the first water wash required one 1 5 ml portion of salt solution the bicarbonate wash two 2 and the last water wash five 5 with careful separation the water content by kf was reduced to less than 1 the volume of aqueous.