Synthesis method of gastrodin
A synthesis method and technology of gastrodin, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., to achieve the effects of low cost, stable quality, safe and easy operation
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[0046] Example 1
[0047] Put 300g of ethyl acetate into the reactor and then put 50g of potassium triacetoxyborohydride, and then put 100g of 4-formylphenyl-2,3,4,6-tetra-0-acetyl-β-D-pyran Glucoside, the temperature is controlled at 20 to 30 ℃ to keep the reaction, take a sample and use TLC to monitor the reaction, the reaction is completed for 1 hour, the reaction solution is added to 300ml of water to quench, then the upper organic phase is separated, and the organic phase is concentrated to a solid under vacuum Then add 300g methanol and 22g diethylamine to reflux and react for 2 hours, take a sample and monitor the reaction with TLC. After the reaction is complete, add 10g activated carbon to decolorize for 10 minutes, filter, concentrate the filtrate to one-third of the original volume, and add to the reaction solution Add 300g of acetone to the mixture, stir and crystallize for 1 hour, filter to obtain 70g of warm gastrodin, and dry at 70℃ to obtain 55g of gastrodin. The...
Example Embodiment
[0048] Example 2
[0049] Put 300g ethyl acetate into the reactor and then 50g sodium triacetoxyborohydride, and then put 100g 4-formylphenyl-2,3,4,6-tetra-0-acetyl-β-D-pyran The temperature of the glucoside was controlled at 20 to 30°C and the reaction was kept warm. Samples were taken and the reaction was monitored by TLC. The reaction was completed in 2 hours. The reaction solution was added to 300ml of water to quench, and then the upper organic phase was separated. The organic phase was concentrated to a solid under vacuum. Then add 300g methanol and 22g diethylamine to reflux and react for 2 hours, take a sample and monitor the reaction with TLC. After the reaction is complete, add 10g activated carbon to decolorize for 10 minutes, filter, concentrate the filtrate to one third of the original volume, and add it to the reaction solution Add 300 g of acetone, stir and crystallize for 1 hour, filter to obtain 65 g of gastrodin, and then dry at 70°C to obtain 52 g of gastrodin....
Example Embodiment
[0050] Example 3
[0051] Put 200g ethyl acetate into the reactor, then 50g potassium triacetoxyborohydride, and then 100g 4-formylphenyl-2,3,4,6-tetra-0-acetyl-β-D-pyran The temperature of the glucoside was controlled at 20 to 30°C and the reaction was kept warm. Samples were taken and the reaction was monitored by TLC. The reaction was completed within 1.5 hours. The reaction solution was added to 300ml of water to quench, and then the upper organic phase was separated. The organic phase was concentrated to a solid under vacuum. Then add 300g methanol and 22g diethylamine to reflux and react for 2 hours, take a sample and monitor the reaction with TLC. After the reaction is complete, add 10g activated carbon to decolorize for 10 minutes, filter, concentrate the filtrate to one third of the original volume, and add it to the reaction solution Add 300g of acetone, stir and crystallize for 1 hour, filter to obtain 68g of gastrodin, and then dry at 70℃ to obtain 53g of gastrodin. ...
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