Method for synthesizing methyl p-bromo-methyl benzoate through channelization and reaction device

A technology for methyl bromomethyl bibenzoate and methyl methyl bibenzoate, which is applied in the field of pipeline synthesis of methyl p-bromomethyl bibenzoate and its reaction device, and can solve the problem of inefficient utilization of bromine atoms. Advanced problems, to achieve the effect of strong industrial application value, less by-products, and high production efficiency

Inactive Publication Date: 2020-11-24
ZHEJIANG KINGLYUAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0017] In summary, the first two methods in the above-mentioned methods have the problem of recycling bromine atom carrier molecules, while the latter two methods have the disadvantage of low utilization rate of bromine atoms

Method used

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  • Method for synthesizing methyl p-bromo-methyl benzoate through channelization and reaction device
  • Method for synthesizing methyl p-bromo-methyl benzoate through channelization and reaction device
  • Method for synthesizing methyl p-bromo-methyl benzoate through channelization and reaction device

Examples

Experimental program
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Effect test

Embodiment 1

[0050] Reactor such as figure 1 shown. The length of the reactor pipe is 40m, the diameter is 3mm, the pipe material is Teflon, and the light source is a 405nm purple LED lamp.

[0051] First open the semiconductor temperature control box 10 precooling pipelines, the temperature is set at 15°C, add 150mL ice water and 10 grams of sodium carbonate in the receiving tank 15; After dichloromethane is stored in the methyl p-methyl bibenzoate liquid storage tank 1, add a sufficient amount of 40% hydrobromic acid in the hydrobromic acid aqueous solution liquid storage tank 2, add a sufficient amount of in the hydrogen peroxide aqueous solution liquid storage tank 3 30% hydrogen peroxide; after turning on the light source, start each pump to pump the material, adjust the pump speed to make the molar ratio of methyl p-methylbibenzoate:hydrogen bromide:hydrogen peroxide controlled at 1:1.1:1.2, and control the reaction temperature at 35~ 38°C, the reaction time is 15min; after the rea...

Embodiment 2

[0053] The structure of the reaction device is as figure 1 As shown, the length of the reactor pipe is 40m, the diameter is 3mm, the pipe material is Teflon, and the light source is a 475nm blue LED lamp.

[0054] First open the pre-cooling pipeline of the semiconductor temperature control box, the temperature is set at 16°C, add 150mL of ice water and 10 grams of sodium carbonate in the receiving tank 15; After the ethyl ester is stored in the methyl p-methylbibenzoate liquid storage tank 1, add a sufficient amount of 40% hydrobromic acid in the hydrobromic acid aqueous solution liquid storage tank 2, add a sufficient amount of 30% hydrobromic acid in the hydrogen peroxide aqueous solution liquid storage tank 3 % hydrogen peroxide; after turning on the light source, start each pump to pump the material, adjust the pump speed to make methyl p-methyldibenzoate: hydrobromic acid: hydrogen peroxide molar ratio be controlled at 1:1.2:1.4, control the reaction temperature at 36~40 ...

Embodiment 3

[0056] The structure of the reaction device is as figure 1 As shown, the length of the reactor pipe is 40m, the diameter is 3mm, the pipe material is Teflon, and the light source is a 565nm yellow-green LED lamp.

[0057] First open the pre-cooling pipeline of the semiconductor temperature control box, the temperature is set at 16 ° C, add 200 mL of ice water and 10 grams of sodium carbonate in the receiving tank 15; Finally, it is stored in the methyl p-methyl bibenzoate liquid storage tank 1, a sufficient amount of 40% hydrobromic acid is added in the hydrobromic acid aqueous solution liquid storage tank 2, and a sufficient amount of 30% hydrogen peroxide is added in the hydrogen peroxide aqueous solution liquid storage tank 3 After turning on the light source, start each pump to pump the material, adjust the speed of each pump to make methyl p-methylbibenzoate: hydrobromic acid: hydrogen peroxide mol ratio is controlled at 1:1.3:1.5, and the control reaction temperature is ...

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Abstract

The invention discloses a method for synthesizing methyl p-bromo-methyl benzoate through channelization and a reaction device. The method comprises the steps: methyl p-methyl benzoate is taken as a raw material, bromine generated by oxidizing hydrobromic acid through hydrogen peroxide is taken as a bromination reagent, materials are continuously input into an efficient mixer through a metering pump to be mixed and then enter a pipeline reactor, a reactant is subjected to a bromination reaction in the pipeline reactor through temperature control and illumination and then collected by a receiving tank, and after an obtained reaction solution is quenched, separated, dried, concentrated and subjected to recrystallization purification, a pure methyl p-bromo-methyl benzoate product is obtained.The bromination reaction has the high bromine atom utilization rate, fewer byproducts and fewer solid wastes, and conforms to the concept of green chemistry; and a continuous pipeline reaction is goodin safety, short in reaction time and high in production efficiency, and has industrial production and application value.

Description

technical field [0001] The invention discloses a pipeline synthesis method of methyl p-bromomethyl bibenzoate and a reaction device thereof. Background technique [0002] Telmisartan is a new type of antihypertensive drug, a specific angiotensin II receptor (AT I type) antagonist, used for the treatment of essential hypertension. The alternative angiotensin II receptor binds with high affinity to the ATI receptor subtype (the known site of action of angiotensin II). Administration of 80 mg telmisartan in humans can almost completely inhibit the increase in blood pressure caused by angiotensin Ⅱ, and the inhibitory effect can last for 24 hours and can still be detected at 48 hours. Through the treatment of telmisartan, the risk of myocardial infarction, stroke or death caused by cardiovascular disease can be reduced. Methyl p-bromomethylbibenzoate is an important building block for the synthesis of telmisartan, and the efficient and convenient synthesis of this intermediate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/12B01F13/10C07C67/307C07C69/78
CPCB01J19/122B01J19/0046C07C67/307B01F33/80B01F33/8362C07C69/78
Inventor 盛凯蔓张晓伟唐雄峰金红卫章治国罗洪根
Owner ZHEJIANG KINGLYUAN PHARMA
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