Preparation method of high-purity D-penicillamine
A penicillamine, high-purity technology, applied in the field of medicine, can solve the problems of difficulty, easy environmental pollution, high toxicity of amines, etc., and achieves the effects of low production cost, simple process and high yield
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Embodiment 1
[0021] Take 100.0 g of penicillin G industrial potassium salt, dissolve it in 1500 ml of water, add 26.9 ml of 40% aqueous sodium hydroxide solution with a molar ratio of 1 / 1, stir at 30°C for 50 minutes, add 87.8 ml of 30% sulfuric acid with a molar ratio of 1 / 1 , Stir evenly and filter to obtain penicillazole acid. Add 500 ml of n-butanol, heat and reflux in an oil bath at 126°C for 20 hours, after decarboxylation, add phenylhydrazine at a molar ratio of 1 / 1.5, protect with nitrogen, heat and reflux at 130°C for 1 hour, drop to 20-25°C, filter, add water to the crude product Just dissolve to obtain a saturated solution, add 5 times the volume of water in ethanol, crystallize at 0-5°C, filter and dry to obtain 25.3 g of D-penicillamine (theoretically converted to 40 g), the yield is 63.3%, and D-penicillamine The content of mycamine is 99.4%, and the impurity dithiopenicillamine is 0.5%.
Embodiment 2
[0023] Take 100.0 g of penicillin G industrial sodium salt, dissolve it in 900 ml of water, add 56.2 ml of 20% aqueous sodium hydroxide solution, stir at 20°C for 50 minutes, add 55.1 ml of 50% sulfuric acid, stir evenly, and filter to obtain penicillazole acid. Add 500 ml of methanol, heat and reflux at 66°C for 11 hours, after decarboxylation, add phenylhydrazine at a molar ratio of 1 / 1.1, protect with nitrogen, heat and reflux at 68°C for 2 hours, lower to 20-25°C, filter, add water until the crude product just dissolves, and get Saturated solution, add methanol 3 times the volume of water, crystallize at 0-5 ° C, filter and dry to obtain 28.4 g of D-penicillamine, the yield is 67.9%, the content of D-penicillamine is 99.1%, and the impurity dithiopenicillamine is 0.8%.
Embodiment 3
[0025] In the production process of penicillin fermentation and extraction, 141.7 g (content 73.6%) of the crude penicillin V potassium salt obtained by recovering the mother liquor was used to replace the penicillin G industrial potassium salt in Example 1, and the others were the same as in Example 1 to obtain D-penicillamine 24.3 g, the content is 99.1%, the impurity dithiopenicillamine is 0.8%, and the yield is 60.7%.
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