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Preparing method of 3',4',7'-troxerutin

A technology of trihydroxyethyl rutin and rutin, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve problems such as methanol waste, reduce waste generation, simple production process, and reduce waste. The effect of reducing the by-products of butyoxyhydrolysis

Active Publication Date: 2017-04-26
CHONGQING BEISHENG PHARMA TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Aiming at the defects in the prior art, the present invention provides a simple, safe, environmentally friendly and cost-effective preparation method of 3',4',7-trihydroxyethyl rutin, which can also solve the waste of methanol in the extraction of crude products The problem

Method used

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  • Preparing method of 3',4',7'-troxerutin

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Experimental program
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Effect test

Embodiment 1

[0035] Under room temperature, 200kg of reaction solvent water is pumped into the reaction tank, then 61kg of rutin is dropped into, and the catalyst potassium hydroxide solution (containing potassium hydroxide 8.14kg) is added dropwise under the nitrogen protection stirring condition, and then chloroethanol 24.4kg is slowly added under the liquid surface. kg, heated up to 65°C, reacted at constant temperature for 4 hours, then added potassium hydroxide solution (containing potassium hydroxide 4.1kg), continued to react for 16 hours, then took samples, and after the reaction was completed by HPLC, cooled to 18°C ​​in an ice-water bath, nitrogen The pH was adjusted to 4.5 with hydrochloric acid under protection. Distill the reaction liquid to dryness under reduced pressure, add 6 times of methanol with the solid mass obtained by distillation under reduced pressure, stir and heat to reflux at 65°C for half an hour, cool down to 20°C and crystallize for 10 hours, centrifuge and fi...

Embodiment 2

[0037] Under room temperature, 2000kg of reaction solvent water is pumped in the reaction tank, then drop into rutin 610kg, drip catalyst potassium hydroxide solution (containing potassium hydroxide 82kg) under nitrogen protection stirring condition, then slowly add chloroethanol 244kg under the liquid level, Raise the temperature to 67°C, react at constant temperature for 4.5 hours, then add potassium hydroxide solution (containing potassium hydroxide 40kg), continue to react for 18 hours, then take samples, after the HPLC detection is complete, cool to 20°C in an ice-water bath, adjust with hydrochloric acid under nitrogen protection pH to 5.2. Distill the reaction liquid to dryness under reduced pressure, add 5 times of the solid mass of methanol obtained by distillation under reduced pressure, stir, heat to 68°C and reflux for 40 minutes, cool down to 22°C and crystallize for 11 hours, and centrifuge to obtain 3',4',7-trihydroxy Ethyl rutin crude product, the obtained moth...

Embodiment 3

[0039]Under room temperature, 2000kg of reaction solvent water is pumped in the reaction tank, then drop into rutin 610kg, drip catalyst potassium hydroxide solution (containing potassium hydroxide 79kg) under the nitrogen protection stirring condition, then slowly add chloroethanol 246kg under the liquid level, Raise the temperature to 68°C, react at constant temperature for 4 hours, then add potassium hydroxide solution (containing potassium hydroxide 42kg), continue to react for 20 hours, then take samples, after the HPLC detection is complete, cool to 18°C ​​in an ice-water bath, adjust with hydrochloric acid under nitrogen protection pH to 6. Distill the reaction liquid to dryness under reduced pressure, add 4 times of methanol with the solid mass obtained by distillation under reduced pressure, stir and heat to 75°C for reflux for 45 minutes, cool down to 24°C for crystallization for 12 hours, and centrifuge to obtain 3',4',7-trihydroxy Ethyl rutin crude product, the obt...

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Abstract

The invention relates to a preparing method of 3',4',7'-troxerutin. The provided preparing method of 3',4',7'-troxerutin comprises the steps of mixing water and rutin at 10-30 DEG C, dropwise adding a catalyst potassium hydroxide solution under the condition of nitrogen protection stirring, slowly adding ethylene chlorohydrin, increasing the temperature to 60-70 DEG C, conducting a thermostatic reaction for 4-5 hours, and then adding potassium hydroxide to continue the reaction for 15-20 hours; the 3',4',7'-troxerutin is obtained after purification and refinement. The 3',4',7'-troxerutin prepared through the method is simple in production technology, and little oxidation hydrolysis by-product is generated, and the 3',4',7'-troxerutin is high in yield. By adopting water as a solution, purification solution formaldehyde can be recycled and utilized at the same time, thus the cost is sharply saved in large-scale production, meanwhile, the generation of waste materials is reduced, and economy and environmental friendliness of production is achieved.

Description

technical field [0001] The invention belongs to the field of drug synthesis, and in particular relates to a preparation method of 3',4',7-trihydroxyethyl rutin. Background technique [0002] Troxerutin is a mixture of semi-synthetic flavonoids made by hydroxyethylation of rutin, which can inhibit the aggregation of red blood cells and platelets, prevent thrombosis, increase the oxygen content in the blood, improve blood microcirculation, and promote angiogenesis to enhance collateral circulation. Furthermore, troxerutin belongs to the general name of hydroxyethyl troxerutin, including monohydroxyrutin, dihydroxyrutin, trihydroxyrutin, tetrahydroxyrutin, among which 3',4',7- Trihydroxyethyl rutin, synthetic raw material rutin (English name Rutin) is also known as rutin, vitamin P, purple quercetin, rutin, rutin powder, lutong, luotong, purple rutin, etc., its CAS number It is 153-18-4, and its molecular structure is as follows: [0003] [0004] Because of its wide rang...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/00
CPCC07H1/00C07H17/07
Inventor 潘先文彭磊夏涛
Owner CHONGQING BEISHENG PHARMA TECH CO LTD
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