Synthetic method of PHBA
A technology of phthaloylaminobutyric acid and its synthesis method, which is applied in the direction of organic chemistry, can solve the problems of high energy consumption, environmental pollution, and high cost, and achieve the effects of low preparation cost, less pollution of "three wastes" and stable quality
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Embodiment 1
[0035] A kind of synthetic method of (S)-alpha-hydroxyl-gamma-N-phthaloylaminobutyric acid, comprises the following steps:
[0036] (1) Preparation of (S)-γ-butyrolactone
[0037] Add 600g of water into the reaction bottle, add 330g of hydrochloric acid and 147g of L-glutamic acid (purified according to the content) in turn under stirring, after dissolving, slowly add NaNO 2 solution (103.5g NaNO 2, 400g water preparation), controlled within 3 to 5 hours (due to the exothermic reaction, it is difficult to keep the cooling environment consistent each time, and the dropping time is also difficult to control at a specific time, and the dropping within this time period will not affect the reaction ) was added, the dropwise addition was completed, and the reaction was continued at 40 to 45°C for 0.5 hours; the reaction was stopped, water was evaporated under reduced pressure, cooled to room temperature, the residue was extracted with 65g × 2 ethyl acetate, and the ethyl acetat...
Embodiment 2
[0047] A kind of synthetic method of (S)-alpha-hydroxyl-gamma-N-phthaloylaminobutyric acid, comprises the following steps:
[0048] (1) Preparation of (S)-γ-butyrolactone
[0049] Add 600g of water into the reaction bottle, add 541g of sulfuric acid and 147g of L-glutamic acid (purified according to the content) in sequence under stirring, after dissolving, slowly add NaNO dropwise 2 solution (103.5g NaNO 2 , prepared with 400g water), control the addition in 3-5 hours, dropwise, continue the reaction at 40-45°C for 0.5 hours; stop the reaction, distill off the water under reduced pressure, cool to room temperature, and use 65g×2 ethyl acetate for the residue Extracted, evaporated ethyl acetate under reduced pressure to obtain (S)-γ-butyrolactone 140g, content 89.1%, yield 95.9%;
[0050] (2) Preparation of (S)-α-hydroxyglutarate monoamide sodium salt
[0051] Cool 314.3g of 25% ammonia solution to below 10°C, add (S)-γ-butyrolactone 135g in batches under stirring, ...
Embodiment 3
[0059] A kind of synthetic method of (S)-alpha-hydroxyl-gamma-N-phthaloylaminobutyric acid, comprises the following steps:
[0060] (1) Preparation of (S)-γ-butyrolactone
[0061] Pump 204 kg of pure water and 32.7kg of 2N sulfuric acid into the reaction kettle through the bottom valve, add 52.4kg of L-glutamic acid under stirring, add dropwise 35.2kg of sodium nitrite aqueous solution, and keep the reaction at 40-45°C after the dropwise addition 2 hours. Concentrate under reduced pressure until no fraction distills out, add 55kg of ethyl acetate, extract, concentrate the extract until dry to obtain (S)-γ-butyrolactone 60.0Kg content 89.1%, yield 95.9%;
[0062] (2) Preparation of (S)-α-hydroxyglutarate monoamide sodium salt
[0063] Put 400Kg of 25% ammonia solution into the reaction kettle, lower the temperature to below 10°C, add 60Kg of (S)-γ-butyric acid lactone in batches under stirring, and continue to react for 3 to 5 hours until the lactone is completely dissolv...
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