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Utilize the method for solid acid-base catalyzed synthesis of vinpocetine

A technology of acid-base catalysis and solid acid, which is applied in the chemical industry, can solve the problems of a large amount of acid-base wastewater, consume large acid-base, and environmental protection pressure, and achieve the effects of promoting esterification and dehydration reactions, good environmental protection, and promoting synthesis

Active Publication Date: 2016-07-06
成都上交致远生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production process mostly involves expensive catalysts such as 2-fluoro-1,3,5,trinitrobenzene, Ti(OEt), and the use of acetonitrile as a solvent is highly toxic and environmentally friendly
It has been found that vincamine can be hydrolyzed by sodium hydroxide to obtain vincamine, and then vincamine is dehydrated and esterified with concentrated sulfuric acid to obtain vinpocetine with a total yield of 90%. However, the above-mentioned liquid acid-base catalyzed production process It needs to consume a lot of acid and alkali, produce a lot of acid and alkali wastewater, and the pressure on environmental protection is great

Method used

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  • Utilize the method for solid acid-base catalyzed synthesis of vinpocetine
  • Utilize the method for solid acid-base catalyzed synthesis of vinpocetine

Examples

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Effect test

Embodiment 1

[0028] The present embodiment relates to a kind of method utilizing solid acid-base catalysis to synthesize Vinpocetine, and described method comprises the steps:

[0029] Step 1, solid alkali hydrolysis: vincamine and dehydrated alcohol are 1:10 to prepare vincamine ethanol solution by weight ratio, and described vincamine ethanol solution is sent into aluminoxomonosodium (particle size is 0.1mm) hydrolysis column for hydrolysis reaction, the column temperature is 60°C.

[0030] Step 2, molecular sieve dehydration: pass the hydrolyzed vincamine ethanol solution through a 3A molecular sieve dehydration column at a flow rate of 30 ml / hour to perform a dehydration reaction, and the column temperature is 60°C.

[0031] Step 3, dehydration and esterification of solid acid: the feed liquid after dehydration enters at a rate of 30 ml / hour to contain 1% 3A molecular sieve packing and a particle size of 0.1 mm solid acid SO 4 2- / TiO 2 -Fe 2 o 3 Fill the solid acid dehydration es...

Embodiment 2

[0035] The present embodiment relates to a kind of method utilizing solid acid-base catalysis to synthesize Vinpocetine, and described method comprises the steps:

[0036] Step 1, solid alkali hydrolysis: vincamine and dehydrated alcohol are 1:20 to prepare vincamine ethanol solution by weight ratio, and described vincamine ethanol solution is sent into aluminoxomonosodium (particle size is 2mm) hydrolysis column for hydrolysis reaction; column temperature is 180°C;

[0037] Step 2, molecular sieve dehydration: the hydrolyzed vincamine ethanol solution is passed through a 3A molecular sieve dehydration column at a flow rate of 3 liters per hour, and the column temperature is 180°C.

[0038] Step 3, dehydration and esterification of solid acid: the feed liquid after dehydration enters at a speed of 3 liters / hour to contain 10% 3A molecular sieve packing and a particle size of 2 mm solid acid SO 4 -2 / ZrO 2 Fill the solid acid dehydration esterification column with solid acid...

Embodiment 3

[0042] The present embodiment relates to a kind of method utilizing solid acid-base catalysis to synthesize Vinpocetine, and described method comprises the steps:

[0043] Step 1, solid alkali hydrolysis: vincamine and absolute ethanol are prepared vincamine ethanol solution at a weight ratio of 1:20, and the vincamine ethanol solution is fed into monosodium aluminoxide, dialuminum oxide with a flow rate of 2 liters / hour. The mixture of sodium (particle size is 1mm) is hydrolyzed on the column, and the hydrolysis reaction is carried out, and the column temperature is 100°C.

[0044] Step 2, molecular sieve dehydration: the hydrolyzed vincamine ethanol solution is passed through a 3A molecular sieve dehydration column at a flow rate of 2 liters per hour, and the column temperature is 100°C.

[0045] Step 3, dehydration and esterification of solid acid: the feed liquid after dehydration enters at a speed of 2 liters / hour to contain 20% 3A molecular sieve packing and a particle s...

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Abstract

The invention discloses a method for catalyzed synthesis of vinpocetine by using solid acid and alkali. The method comprises the following steps: 1, carrying out hydrolysis of solid alkali, namely feeding a vincamine ethanol solution to a solid alkali hydrolysis column to carry out a hydrolysis reaction; 2, dewatering by a molecular sieve, namely carrying out a dewatering reaction on the hydrolyzed vincamine ethanol solution through a molecular sieve dewatering column; and 3, dewatering and esterifying solid acid, namely feeding the dewatered feed liquid to a solid acid dewatering and esterifying column to carry out solid acid dewatering and esterifying. Strong alkali instead of sodium hydroxide is adopted to catalyze hydrolysis of vincamine; and solid strong acid instead of concentrated sulfuric acid is used for carrying out dewatering and esterifying, so as to obtain the vinpocetine. A catalyst used by the method can be conveniently separated from a product, so that the production cost is reduced. According to the method disclosed by the invention, no acid-alkali wastewater is generated in the production process; the method is environment-friendly and more suitable for industrial production, and can be repeatedly used; the production cost can be effectively reduced; and the used solid acid and alkali are free of corrosion on equipment, environment-friendly, and do not generate acid-alkali wastewater.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for synthesizing vinpocetine by solid acid-base catalysis. Background technique [0002] Vinpocetine is a cerebral vasodilator that can inhibit phosphodiesterase activity, selectively increase cerebral blood flow, increase cerebral oxygen consumption, and improve cerebral metabolism. It is mainly used clinically to improve sequelae of cerebral infarction, sequelae of cerebral hemorrhage, cerebral Various symptoms induced by arteriosclerosis, etc. [0003] At present, Vinpocetine is mainly produced through a chemical semi-synthesis process using vincamine as a raw material. The production process mostly involves expensive catalysts such as 2-fluoro-1,3,5,trinitrobenzene and Ti(OEt), and the use of acetonitrile as a solvent is highly toxic and poor in environmental protection. It has been found that vincamine can be hydrolyzed by sodium hydroxide to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D461/00
Inventor 苗志奇陈榕华朱闪烁唐克轩于湘莉
Owner 成都上交致远生物科技有限公司
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