Diethyl L-glutamate hydrochloride synthesis
- Product Name:Diethyl L-glutamate hydrochloride
- CAS Number:1118-89-4
- Molecular formula:C9H18ClNO4
- Molecular Weight:239.7
64-17-5
56-86-0
1118-89-4
To a 500 mL four-necked round-bottomed flask equipped with a mechanical stirrer, a thermometer and a reflux condenser tube (connected to a 30% aqueous sodium hydroxide solution absorption system), 300 g of ethanol, 14.7 g (0.10 mol) of L-glutamic acid, and 25.0 g (0.08 mol) of triphosgene were added sequentially. The reaction mixture was heated to 70-75°C and maintained at this temperature with stirring for 5 hours. Upon completion of the reaction, the system was cooled to 20-25°C and the hydrogen chloride gas generated in the system was removed by nitrogen displacement, a process that lasted for 30 minutes. Subsequently, the excess triphosgene and ethanol were recovered by distillation. To the residue, 100 mL of methyl tert-butyl ether was added for pulping, and after filtration and drying, 23.5 g of the white solid product L-glutamic acid diethyl ester hydrochloride was obtained. The product was analyzed by liquid chromatography with 99.7% purity and 98.0% yield.
Yield:1118-89-4 98%
Reaction Conditions:
Stage #1:ethanol;L-glutamic acid with bis(trichloromethyl) carbonate at 70 - 75; for 5 h;
Stage #2: with hydrogenchloride at 20 - 25; for 0.5 h;
Steps:
3 Example 3:Preparation of L-glutamic acid diethyl ester hydrochloride (III2)
To a 500 ml four-necked flask equipped with a stirrer, a thermometer and a reflux condenser (connected with 30% aqueous sodium hydroxide solution), 300 g of ethanol was added.14.7 g (0.10 mol) L-glutamic acid, 25.0 g (0.08 mol) triphosgene, Heat, react at 70-75°C for 5 hours, cool to 20-25°C,Hydrogen chloride gas in the nitrogen substitution system was replaced 30 minutes later.Distillation recovers excess triphosgene and ethanol, then adds 100 to the residueMethyl tert-butyl ether, beaten, filtered and dried to give 23.5 g of a white solidL-glutamic acid diethyl ester hydrochloride, liquid purity 99.7%, yield 98.0%.
References:
Xin Fa Pharmaceutical Co., Ltd.;Qi Yuxin;Qu Hu;Wang Baolin;Xu Xin;Ju Lizhu;Li Xinfa CN107602436, 2018, A Location in patent:Paragraph 0051; 0052
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