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Glycine (lg, 13.3 mmol) was dissolved in isopropanol (10 mL) at 0C. SOCl2 (1.93 mL, 26.6 mmol) was added dropwise. The mixture was stirred at reflux overnight. After cooling, the solvent was evaporated under reduced pressure and hexane was added at 0C. The suspension was filtered to afford the product (1.76 g, 86%) as a white solid. NMR (300 MHz, MeOD) delta 5.13 (hept, J = 6.3 Hz, 1H, (CH3)2CHO), 3.81 (s, 2H, CH2), 1.32 (s, 3H, (CH3 2CHO . 1.30 (s, 3H, iCH3}2CHO). 13C NMR (75 MHz, MeOD) delta 168.0 (C), 71.7 ((CH3)2CHO), 41.2 (CH2), 21.9 ((CH3 2CHO . HRMS [M+H]+ C5H12NO2: Calcd. 1 18.0858 found 1 18.0863.
In the 100ml three-necked flask, 30ml of isopropyl alcohol was added, and then 2.6ml of SOCl2 was added dropwise. The temperature of the dropping process was controlled at -10C to 0C, and the reaction was continued under stirring for 1 hour after the addition. 0.75g of glycine was added, and the mixture was warmed naturally to react at room temperature for 3h. The solution turned into a white emulsion, and the mixture was heated at reflux for 4 h until the solid completely disappeared. After removal of excess ethanol and SOCl2 under reduced pressure, a yellow viscous liquid was obtained.
With thionyl chloride; at 0 - 20℃; for 4h;
General procedure: A solution of thionyl chloride (4.5ml, 0.06mol) in anhydrous ethanol (30ml, 0.52mol) was added to glycine (3.3g, 0.02mol) with stirring at 0C for 1h and then at room temperature for another 3h. L-ethyl glycinate hydrochloride was synthesized after removal of the solvent.
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