Method for synthesizing theanine
A synthesis method and theanine technology, applied in chemical instruments and methods, preparation of carboxylic acid amides, preparation of organic compounds, etc., can solve the problems of poor selectivity, slow reaction speed, low yield and the like
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example 1
[0074] Weigh in a 1000ml three-necked bottle, add 60g of L-glutamic acid, 600ml of absolute ethanol, cool to 10°C under stirring, add 30ml of concentrated sulfuric acid dropwise, after the dropwise reaction at room temperature for 8 hours, add dropwise Triethylamine was neutralized, filtered after cooling, and the filter cake was dried to obtain 50 grams of L-glutamic acid-γ-ethyl ester with a yield of 70%.
[0075] In a 1000ml three-necked flask, add 40g of L-glutamic acid-γ-ethyl ester, add 600ml of ethanol aqueous solution, add 60g of sodium bicarbonate, dissolve and cool to 10°C, add 40ml of acetic anhydride dropwise, and dropwise Afterwards, react at room temperature for 3 hours, concentrate and desalinate to obtain L-N-acetyltheanine solution, add 300 ml of 70% ethylamine aqueous solution, stir the reaction until the ammoniation reaction is complete, and obtain L-N-acetyltheanine solution.
[0076] The L-N-acetyltheanine solution is concentrated, and the solution is chec...
example 2
[0078] Example 1 Weigh in a 1000ml three-necked bottle, add 60g of L-glutamic acid, 500ml of n-butanol, stir and cool to below 10°C, add 30ml of concentrated sulfuric acid dropwise, after the dropping, react at room temperature for 12 After 1 hour, triethylamine was added dropwise until neutral, filtered after cooling, and the filter cake was dried to obtain 66.6 g of L-glutamic acid-γ-n-butyl ester with a yield of 80%.
[0079] In a 1000 ml three-necked flask, add 40 g of L-glutamic acid-γ-n-butyl ester, add 400 ml of ethanol aqueous solution, add 50 g of sodium bicarbonate, dissolve and cool below 10°C, add dropwise 50 ml of acetic anhydride, After dropping, react at room temperature for 2 hours, concentrate and desalt to obtain L-N-acetylglutamic acid-γ-n-butyl ester solution, add 400 ml of 70% ethylamine aqueous solution, stir and react until the ammoniation reaction is complete, and obtain L-N-acetylglutamate acid solution.
[0080] The L-N-acetyltheanine solution is con...
example 3
[0082] In a 1000 ml three-necked flask, add 60 grams of L-glutamic acid and 600 ml of absolute ethanol, cool to 10°C under stirring, add 30 ml of concentrated sulfuric acid dropwise, and react at room temperature for 8 hours, add triethyl ether dropwise The amine was neutralized, filtered after cooling, and the filter cake was dried to obtain 50 g of L-glutamic acid-γ-ethyl ester with a yield of 70%.
[0083] In a 1000ml three-neck flask, add 40g of L-glutamic acid-γ-ethyl ester, add 200ml of water, add 40g of sodium bicarbonate, dissolve and cool to 10°C, add 15ml of benzoyl chloride dropwise, and dropwise Afterwards, react at room temperature for 2 hours, concentrate and desalinate to obtain L-N-benzoylglutamic acid-γethyl ester solution, add 400 ml of 70% ethylamine aqueous solution, stir the reaction until the ammoniation reaction is complete, and obtain L-N-benzoylglutamate acid solution.
[0084] The L-N-benzoyltheanine solution is concentrated, and the solution is chec...
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