Method for preparing 5-aminolevulinic acid hydrochloride
A technology of aminolevulinic acid hydrochloride and hydrochloric acid solution, which is applied in the fields of medicinal chemistry and medicinal chemistry synthesis, can solve the problems of complex technological process, many raw materials and production equipment, long routes and the like, and achieves simple and continuous operation, low cost, high yield effect
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Embodiment 1
[0041]
[0042] Take I-1 (1Kg, 7.6mol), succinic anhydride (0.763Kg, 7.6mol), suspend in 2L of methanol, add sodium methoxide (0.41Kg, 7.6mol), heat to 60°C and reflux for 0.5~2h. After the complete reaction was detected by GC, the temperature was cooled to below 10°C in an ice bath, dilute hydrochloric acid (900 mL, 7.6 mol) was slowly added dropwise, methyl acetate (2 L) was added, and the layers were separated. After discarding the water phase, continue to add concentrated hydrochloric acid (364mL, 7.6mol) dropwise, heat to reflux for 0.5-2h, recover methanol during the process, control the temperature at 60°C-90°C, the temperature will increase as the reaction progresses, and control the pH to 1.0~3.5. After the complete reaction was detected by GC, water and generated acetic acid were distilled off under reduced pressure. After the solvent was evaporated, ethyl acetate (3 L) was added to crystallize, filtered, and dried to obtain 1.02 Kg of the product 5-aminolevulini...
Embodiment 2
[0045]
[0046] Take I-2 (1Kg, 7.0mol), succinic anhydride (0.693Kg, 7.0mol), suspend in 2L of ethanol, add sodium ethoxide (0.476Kg, 7.0mol), heat to 70°C and reflux for 3~5h. After the complete reaction was detected by GC, the temperature was cooled to below 10°C in an ice bath, dilute hydrochloric acid (700 mL, 7.0 mol) was slowly added dropwise, ethyl acetate (2 L) was added, and the layers were separated. After discarding the water phase, continue to add concentrated hydrochloric acid (584mL, 7.0mol) dropwise, heat and reflux for 2 to 5 hours after addition, recover ethanol during the process, control the temperature at 70°C to 95°C, and control the temperature as the reaction progresses. The pH is 1.0-3.5. After the complete reaction was detected by GC, water and generated acetic acid were distilled off under reduced pressure, ethyl acetate (3 L) was added to crystallize, filtered, and dried to obtain 0.935 Kg of the product 5-aminolevulinic acid hydrochloride with a ...
Embodiment 3
[0048]
[0049] Take I-3 (1Kg, 4.3mol), succinic anhydride (0.43Kg, 4.3mol), suspend in 2L of tert-butanol, add sodium tert-butoxide (0.42Kg, 4.3mol), heat to 85°C and reflux for 10~ 12h. After the complete reaction was detected by GC, the temperature was cooled to below 10°C in an ice bath, dilute hydrochloric acid (500 mL, 4.3 mol) was slowly added dropwise, ethyl acetate (2 L) was added, and the layers were separated. After discarding the water phase, continue to add concentrated hydrochloric acid (359mL, 4.3mol) dropwise, heat and reflux for 6-8 hours after the addition, recover tert-butanol during the process, control the temperature at 90°C-100°C, and the temperature will increase as the reaction progresses , control the pH to 1.0-3.5. After the complete reaction was detected by GC, water and generated acetic acid were evaporated under reduced pressure, ethyl acetate (3 L) was added to crystallize, filtered, and dried to obtain 0.6 Kg, with a molar yield of 83%.
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