Synthesis
A 500 mL four-necked flask was charged with a 40 wt% aqueous solution of monomethylamine and cooled to 10 ° C in an ice-water bath. Then, while stirring, 1,4-dichloro-2-butanol was added dropwise, and the temperature was controlled at 15 ° C. Then pour the system into an Autoclave, sealed, evacuated to a pressure of 1.0 ± 0.1MPa, while heated to 120 ℃, the reaction was stirred for about 10h. After the reaction was over and cooled to room temperature, the material was discharged, batch-wise added sodium hydroxide was released, and a large amount of methylamine gas, controlling the temperature below 50 ℃, precipitated a lot of white solid, stirred for 1h; filtration, the filtrate layered, the upper organic phase Ethanol And anhydrous magnesium sulfate, stirring 2 ~ 3h; and then filtered, the filtrate was concentrated in vacuo to give a yellow transparent oily liquid, and then vacuum distillation to give colorless and t1-Methyl-3-pyrrolidinol, Yield 64.8%, purity 99.3%.
