to a 100 ml glass receiving flask immersed in an ice water bath to the reaction vial was fed 50 ml of 98 percent hno 3 75 0 g 1 13 mole of hno 3 and 10 ml 8 67 g 0 094 mole of toluene feed rates were 0 60 ml hno 3 min and 0 12 ml toluene min controlled by sage instrument syringe pumps models 351 and 355 reactor content was adjusted to 2 ml by height adjustment of the reactor exit line in the reaction vial for a mean reaction residence time of 2 8 minutes the reactor water bath was maintained at 15 u00b0 u00b1 5 u00b0 c by the periodic addition of ice during reactant addition upon completion of the reactant addition the reactor contents were stirred for 3 minutes then purged to the receiver a total of 83 31 g of pale yellow product solution was obtained distillation of this solution 53 u00b0 c 75 160 mmhg gave 38 75 g of pale yellow acid which analyzed by titration with standardized naoh as 100 percent hno 3 the pot contained 44 21 g of pale yellow solution 0 42 g of hno 3 was lost to the walls of the glassware leaving an estimated 0 43 g of product lost to no 2 vapors during the distillation the pot solution was diluted with 21 72 g of water and extracted with 33 30 g of toluene separation of the layers furnished 48 74 g.