7250-67-1

123-75-1

107-07-3

7250-67-1

The general procedure for the synthesis of N-(2-chloroethyl)pyrrolidine hydrochloride from tetrandrine and 2-chloroethanol was as follows: 165 mL (2 mol) of tetrandrine, 67 mL (1 mol) of 2-chloroethanol, and 200 mL of toluene were added sequentially to a reaction flask. The mixture was heated to reflux temperature and kept reacting for 3 hours. Upon completion of the reaction, the mixture was cooled to room temperature and the solid product was isolated. The solid was collected by diafiltration and the filter cake was washed with 20 mL of toluene. The temperature of the filtrate was controlled at about 75 °C and 200 mL of thionyl chloride was slowly added dropwise. After the dropwise addition was completed, the reaction was continued at reflux for 2 hours. At the end of the reaction, the mixture was cooled to room temperature and subsequently concentrated to dryness under reduced pressure. The resulting residue was recrystallized from anhydrous ethanol to give 105 g of white solid product in 62.3% yield. The melting point of the product was 198-203 °C.