The preparation of 1-pyrrolidine carbonyl chloride is as follows:
In a 1000ml three-necked flask, 400ml of toluene and 54.00g (0.182mol) of triphosgene were added and stirred until dissolved. Then, a mixture of 61.32g (0.606mol) of triethylamine and 50ml of toluene was added dropwise at 5℃. After the addition was complete, the mixture was stirred at the same temperature for 30 minutes. Next, a mixture of 43.03g (0.606mol) of pyrrolidine and 50ml of toluene was added dropwise. After the addition was complete, the mixture was kept at 15℃ for 3 hours. After the reaction was complete, the solid was filtered off. The solid was washed with 50ml of toluene. The filtrate and washings were combined, and the toluene was distilled off under reduced pressure. The resulting product was then distilled under high vacuum to obtain 56.70g of 1-pyrrolidine carbonyl chloride, with a purity of 98.5% and a yield of 69.0%.
