Synthesis
The general procedure for the synthesis of 3-pyrrolidinemethanol from methyl 5-oxopyrrolidine-3-carboxylate is as follows: 2 kg of methyl 5-oxo-3-pyrrolidinecarboxylate is dissolved in 20 liters of tetrahydrofuran, and 1.9 kg of sodium borohydride is added in batches at room temperature. Subsequently, 3.9 kg of boron trifluoride ether solution was slowly added dropwise. After the dropwise addition was completed, the reaction mixture was stirred at room temperature for 10 minutes and then heated to reflux for about 4 hours. Upon completion of the reaction, the reaction was quenched with water and extracted with ethyl acetate. The organic phases were combined and concentrated to give a light yellow oily liquid. This oily liquid was dissolved in ethanol, 500 g of sodium borohydride was added and heated to reflux for 2 hours. At the end of the reaction, the reaction was again quenched with water and extracted with ethyl acetate. The organic phase was washed sequentially with saturated aqueous sodium bicarbonate and saturated brine, and finally the organic phase was concentrated to give 1.2 kg of 3-pyrrolidinemethanol in 86% yield.
