To a 3-neck reflux apparatus equipped with an addition funnel and a thermometer add 88 mL of thionyl chloride, the addition funnel is filled with 58 mL of acetic acid and the condenser is plugged with a calcium chloride drying tube. The RBF is heated at 45°C and with stirring the addition is started for over the course of 30 minutes, thereafter the solution is refluxed for 30 minutes. The solution is then distilled and a fraction of 50-57°C is collected and dried with anhydrous calcium chloride.
Refluxing the solution
Distillation of the solution