A kind of preparation method of 1-2,4-diaminobutyric acid hydrochloride
A technology of diaminobutyric acid hydrochloride and aminobutyric acid is applied in the preparation of carbamic acid derivatives, the preparation of organic compounds, the preparation of cyanide reactions, etc., and can solve the problems of large pollution of three wastes, cumbersome operations, and long routes. Achieve the effect of reducing production costs, reducing three waste emissions, and reducing the use of
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Embodiment 1
[0032] S1: Add 14.6 g of L-glutamine (0.1 mol) to a 500 mL three-necked flask, add 150 mL of water, 10 g of sodium hydroxide (0.25 mol), and after stirring to clarify, add 26.2 g of Boc anhydride (0.12 mol), The reaction was carried out at room temperature overnight, and the dot plate monitoring was completed;
[0033] S2: add 4 grams of sodium hydroxide (0.1 mol), then dropwise add 107 grams of 7% sodium hypochlorite (0.1 mol) at room temperature, and naturally heat up the reaction for half an hour after the completion of the dropwise addition, and the dot plate monitoring reaction is complete;
[0034] S3: The reaction solution is cooled to room temperature, adjusted to pH 5-6 with concentrated hydrochloric acid, desalted with cation resin exchange resin, eluted with 5% ammonia water as eluent, and after the eluent is concentrated, adjusted pH with concentrated hydrochloric acid To 2~3, beating with ethanol to obtain L-2,4-diaminobutyric acid hydrochloride crude product, the...
Embodiment 2
[0036] S1: In a 1000 mL three-necked flask, add 43.8 g of L-glutamine (0.3 mol), add 450 mL of water, 30 g of sodium hydroxide (0.25 mol), and after stirring to clarify, add 78.6 g of Boc anhydride (0.12 mol), The reaction was carried out at room temperature overnight, and the dot plate monitoring was completed;
[0037] S2: add 12 grams of sodium hydroxide (0.1 mol), then dropwise add 321 grams of 7% sodium hypochlorite (0.1 mol) at room temperature, after the completion of the dropwise addition, the reaction is naturally heated for half an hour, and the dot plate monitoring reaction is complete;
[0038] S3: the reaction solution is lowered to room temperature, adjusted pH to 5~6 with concentrated hydrochloric acid, desalted through cation resin exchange resin, eluted with 5% ammonia water as eluent, after the eluent is concentrated, adjusted pH with concentrated hydrochloric acid To 2~3, beating with ethanol to obtain L-2,4-diaminobutyric acid hydrochloride crude product, t...
Embodiment 3
[0040] S1: In a 3000 mL three-necked flask, add 146 g of L-glutamine (1 mol), add 1500 mL of water, 100 g of sodium hydroxide (2.5 mol), and after stirring to clarify, add 262 g of Boc anhydride (0.12 mol), The reaction was carried out at room temperature overnight, and the dot plate monitoring was completed;
[0041] S2: add 40 grams of sodium hydroxide (1 mol), then dropwise add 1070 grams of 7% sodium hypochlorite (1 mol) at room temperature, after the completion of the dropwise addition, the reaction is naturally heated for half an hour, and the dot plate monitoring reaction is complete;
[0042] S3: the reaction solution is lowered to room temperature, adjusted pH to 5~6 with concentrated hydrochloric acid, desalted through cation resin exchange resin, eluted with 5% ammonia water as eluent, after the eluent is concentrated, adjusted pH with concentrated hydrochloric acid To 2~3, beating with ethanol to obtain L-2,4-diaminobutyric acid hydrochloride crude product, the cru...
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