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(1) (R)-3-aminobutyric acid (70 g, 0.68 mol) was dissolved in methanol (1.0L), the ice-water bath was cooled to T <20 C, the dropwise addition of thionyl chloride (97g, 0.82mol), the end of the reaction, the natural reaction overnight, 40-50 C the reaction solution was concentrated to dry oil 99g, yield 95%.
With thionyl chloride; In ethanol; at 0 - 30℃;Inert atmosphere;
Under nitrogen protection,2000 ml of absolute ethanol and 200.0 g (1.94 mol) of R-3-aminobutyric acid (material II) were charged into a 3 L reactor.Stir well; cool down and control temperature to 0-10 C,509.2 g (4.28 mol, 2.2 N) of thionyl chloride was added dropwise.After the dropwise addition, the temperature is raised to 20 to 30 C, and the reaction is kept overnight.The TLC detected until the material II material point disappeared (developing agent: ethyl acetate: methanol = 2:1).After the reaction was completed, distillation under reduced pressure gave a pale yellow concentrate (322.5 g).Yield: 99.2%.
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