Synthesis
The present embodiment is a method for the preparation of 1-ethyl-3-pyrrolidinol, which was carried out as follows: 250 g of 40 wt% aqueous ethylamine solution was added to a 500 mL four-necked flask, cooled to 10 °C, and placed in an ice-water bath. Under stirring conditions, 102 g of 1,4-dichloro-2-butanol was added dropwise, and the temperature was controlled to be about 15 °C. After the dropwise addition was completed in about 15 min, the reaction system was transferred to a 500 mL autoclave, sealed, evacuated to a pressure of 1.0±0.1 MPa, heated to 120±2°C, stirred and reacted for about 10 h. The reaction was monitored by GC until the raw material disappeared. After the reaction was completed, cooled to room temperature, discharged the reaction material, added 110g of sodium hydroxide in batches, taking care to control the temperature below 50°C to release ethylamine gas and precipitate a white solid, and continued stirring for 1h. After filtration, the filtrate was layered, the upper organic phase was taken, 100mL of ethanol and 18g of anhydrous magnesium sulfate were added, and stirred for 2~3h. Filtered again, and the filtrate was concentrated under vacuum to obtain a yellow transparent The filtrate was again filtered and concentrated under vacuum to obtain a yellow transparent oily liquid, and finally 46.7 g of colorless and transparent 1-ethyl-3-pyrrolidinol was obtained by vacuum distillation with a yield of 64.8% and a purity of 99.3% (HPLC).
