Synthesis method of high-purity histamine dihydrochloride
A technology of histamine dihydrochloride and synthesis method, which is applied in the field of synthesis of high-purity histamine dihydrochloride, can solve the problems of limitation and high risk, achieve the reduction of species and content, simple equipment and simple operation Effect
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Embodiment 1
[0039]Add 50 grams of L-histidine, 3 grams of sodium carbonate, 0.25 grams of p-methylacetophenone and 500 grams of dimethyl sulfoxide into a 1000ml three-necked flask equipped with a mechanical stirrer, a thermometer and a reflux device. Replace the air, protect the whole process with nitrogen, heat to 140°C and react for 4 hours, stop the reaction when the histidine content is less than 0.5%, and obtain a golden yellow transparent decarboxylation reaction solution, cool the reaction solution to 50-60°C, filter out insoluble The obtained filtrate was evaporated to remove the solvent under reduced pressure to obtain a viscous substance, add about 150 grams of water to disperse, add about 60 grams of concentrated hydrochloric acid to neutralize to pH 5-6 under ice-bath cooling, after the addition is completed, stir at 20-25 ° C After half an hour, the aqueous solution was extracted three times with about 500 g of ethyl acetate, and the obtained aqueous layer was evaporated to ob...
Embodiment 2
[0047] Add 50 gram L-histidine, 3 gram sodium carbonate, 0.25 gram p-methyl acetophenone and 500 gram embodiment 1 in the 1000ml there-necked flask that mechanical stirring, thermometer, reflux device are housed and reclaim dimethyl sulfoxide , replace the air with vacuum and nitrogen, protect the whole process with nitrogen, heat to 140°C for 4 hours, and stop the reaction when the content of histidine is monitored to be less than 0.5%. ℃, filter out the insoluble matter, evaporate the solvent from the obtained filtrate under reduced pressure to obtain a viscous substance, add about 150 grams of water to disperse, add about 60 grams of concentrated hydrochloric acid to neutralize to pH to 5-6 under ice bath cooling, and dropwise. After stirring at 20-25°C for half an hour, the aqueous solution was extracted three times with about 500 g of ethyl acetate, and the obtained aqueous layer was evaporated to obtain a crude product of histamine dihydrochloride. Add 100 g of absolute ...
Embodiment 3
[0050] Add 50 gram L-histidine, 3 gram sodium carbonate, 0.25 gram p-methyl acetophenone and 500 gram xylene in the 1000ml there-necked bottle that mechanical stirring, thermometer, reflux device are housed, replace air with vacuum and nitrogen, Nitrogen protection throughout the whole process, heating to 140°C for 4 hours, monitoring the histidine content to stop the reaction when it is less than 0.5%, and obtaining a golden yellow transparent decarboxylation reaction solution, cooling the reaction solution to 50-60°C, filtering out insolubles, and obtaining Remove the solvent from the filtrate under reduced pressure to obtain a viscous substance, add about 150 grams of water to disperse, add about 60 grams of concentrated hydrochloric acid to neutralize to pH 5-6 under ice-cooling, after the dropwise addition is completed, stir at 20-25 ° C for half an hour, The aqueous solution was extracted three times with about 500 g of ethyl acetate, and the obtained aqueous layer was ev...
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Description
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Application Information
- IPC
- C07D233/64
- CPC
- C07D233/64
- Inventors
- 唐启明; 吴伟伟