Method for preparing 3-pyrroline based on improved activated zinc powder
A technology for activating zinc powder and pyrroline, applied in the field of medicine, can solve the problems of difficult generation, low product yield, difficult cyclization reaction of diallylamine, etc., and achieves improved reaction activity, high product purity, and easy separation and purification. Effect
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Embodiment 1
[0036] In a clean single-necked flask, add 50ml of solvent dimethyl sulfoxide, 20g (0.3mol) of zinc powder, 99.68g (0.6mol) of terephthalic acid, slowly raise the temperature to 30°C, stir for 1.5h, filter under reduced pressure, The activated zinc powder is obtained. In a clean three-necked flask, add 79.40ml of 30wt% HCl solution, control the temperature at 0°C, stir slowly, add the activated zinc powder, stir quickly, slowly add 5.123ml (0.075mol) of pyrrole dropwise, after the dropwise addition Raise the temperature to 10°C and react for 6h.
[0037] Then filter under reduced pressure to remove the zinc powder, add sodium hydroxide solution dropwise under the condition of water ice bath, adjust the pH to 14, filter under reduced pressure to remove the zinc hydroxide precipitate, extract the filtrate with ether for 3 times, and use the ether extract with anhydrous After drying over sodium sulfate, it was distilled under normal pressure at 35° C., and the remaining distille...
Embodiment 2
[0040] In a clean single-necked flask, add 50ml of solvent dimethyl sulfoxide, 10g (0.15mol) of zinc powder, 81.07g (0.45mol) of 2-methyl-1,4-benzenedicarboxylic acid, slowly raise the temperature to 25°C, and stir After reacting for 1 hour, filter under reduced pressure to obtain activated zinc powder. In a clean three-necked flask, add 238.2ml of 10wt% HCl solution, control the temperature at 0°C, stir slowly, add the activated zinc powder, stir quickly, and slowly add 5.123ml (0.075mol) of pyrrole dropwise. Raise the temperature to 5°C and react for 4h.
[0041] Then filter under reduced pressure to remove the zinc powder, add sodium hydroxide solution dropwise under the condition of water ice bath, adjust the pH to 14, filter under reduced pressure to remove the zinc hydroxide precipitate, extract the filtrate with ether for 3 times, and use the ether extract with anhydrous After drying over sodium sulfate, it was distilled under normal pressure at 35° C., and the remaini...
Embodiment 3
[0043]In a clean single-necked flask, add 100ml of solvent dimethyl sulfoxide, 20g (0.3mol) of zinc powder, 233.02g (1.2mol) of 2,5-dimethyl-1,4-phthalic acid, and slowly heat up to 50 °C, stirred and reacted for 0.5h, and filtered under reduced pressure to obtain activated zinc powder. In a clean three-necked flask, add 47.64ml of 50wt% HCl solution, control the temperature at 0°C, stir slowly, add the activated zinc powder, stir quickly, slowly add 3.415ml (0.05mol) of pyrrole dropwise, after the dropwise addition Raise the temperature to 15°C and react for 5h.
[0044] Then filter under reduced pressure to remove the zinc powder, add sodium hydroxide solution dropwise under the condition of water ice bath, adjust the pH to 14, filter under reduced pressure to remove the zinc hydroxide precipitate, extract the filtrate with ether for 3 times, and use the ether extract with anhydrous After drying over sodium sulfate, it was distilled under normal pressure at 35° C., and the ...
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