Method for synthesizing calcimimetics hydrochloride intermediates by micro passage reactor

A technology of cinacalcet hydrochloride and microchannel reactor, which is applied in the field of synthesizing cinacalcet hydrochloride intermediates in microchannel reactors, can solve the problems of low catalyst recovery times, long reaction time, violent explosion, etc., and achieve stability Effects of on-line production and post-processing, improvement of yield and purity, and reduction of production cost

Inactive Publication Date: 2018-08-03
HEILONGJIANG XINCHUANG BIOLOGICAL TECH DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to solve the problems of low yield, poor purity, risk of violent explosion, degradation caused by long reaction time at high temperature, and low number of times of catalyst recovery and mechanical application in the...

Method used

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  • Method for synthesizing calcimimetics hydrochloride intermediates by micro passage reactor
  • Method for synthesizing calcimimetics hydrochloride intermediates by micro passage reactor
  • Method for synthesizing calcimimetics hydrochloride intermediates by micro passage reactor

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Embodiment 1: the method for microchannel reactor synthesis cinacalcet hydrochloride intermediate

[0042] 1) Weigh 300 g of raw material m-trifluoromethyl cinnamic acid and add it to 3 L of methanol, stir and dissolve, add 10 g of Pd / C catalyst with a mass content of Pd of 10%, fully stir and mix to form material I, and transport material I to micro Preheat in the preheating module 1 of channel reactor, enter the reaction module group of microchannel reactor after preheating;

[0043] 2) Hydrogen is delivered to the reaction module group of the microchannel reactor and step 1) the material I after preheating is reacted in the reaction module group, wherein: adjust the flow rate of the slurry pump so that the flow rate of the material I is 25.0g / min , adjust H 2 The flow rate of the gas flow meter is 350ml / min, the molar ratio of trifluoromethyl cinnamic acid to hydrogen is 1:1.2, the reaction temperature is 80°C, the temperature of the cooling module is 20°C, an...

Embodiment 2

[0044] Embodiment 2: the method for microchannel reactor synthesis cinacalcet hydrochloride intermediate

[0045] This embodiment provides a method for synthesizing a cinacalcet hydrochloride intermediate in a microchannel reactor, and the specific steps are as follows:

[0046] 1) Weigh 300 g of raw material m-trifluoromethyl cinnamic acid and add it to 3 L of ethanol. After stirring and dissolving, add 15 g of Pd / C catalyst with a Pd mass content of 5%, fully stir and mix to form material I, and transport material I to micro The channel reactor is preheated in the preheating module 1, and enters the reaction module group of the microchannel reactor after preheating.

[0047] 2) Hydrogen is delivered to the reaction module group of the microchannel reactor and step 1) reacts with the preheated material I in the reaction module group, wherein: adjust the flow rate of the slurry pump to make the flow rate of the material I 30.0g / min , adjust H 2 The flow rate of the gas f...

Embodiment 3

[0048] Embodiment 3: the method for the synthesis of cinacalcet hydrochloride intermediate by microchannel reactor

[0049] This embodiment provides a method for synthesizing a cinacalcet hydrochloride intermediate in a microchannel reactor, and the specific steps are as follows:

[0050] 1) Weigh 200 g of raw material m-trifluoromethylcinnamic acid and add it to 2L of ethanol, add 20 g of Pt mass content after stirring and dissolving, and add 20 g of Pt / C catalyst with a mass content of 3%, fully stir and mix to form material I, and material I is transported to micro The channel reactor is preheated in the preheating module 1, and enters the reaction module group of the microchannel reactor after preheating.

[0051] 2) Hydrogen is delivered to the reaction module group of the microchannel reactor and step 1) reacts with the preheated material I in the reaction module group, wherein: adjust the flow rate of the slurry pump to make the flow rate of the material I 30.0g / min...

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Abstract

The invention discloses a method for synthesizing calcimimetics hydrochloride intermediates by a micro passage reactor, and belongs to the field of medicine synthesis in organic synthesis. According to the method, p-trifluoromethylcinnamic acid is added into an organic solvent; then, active carbon loaded noble metal catalysts are added; an obtained mixture is used as a first material; the first material is conveyed to a preheating module of the micro passage reactor to be heated; after being preheated, the material enters a reaction module group; hydrogen gas is conveyed to a reaction module group of the micro passage reactor to react with the preheated first material in the step (1) for reaction; reaction liquid flowing out from a temperature lowering module is collected; post treatment is performed to obtain calcimimetics hydrochloride intermediates 3-(3-trifluoromethyl phenyl)propionate. The synthesis method provided by the invention has the advantages that the reaction time can beeffectively shortened; the potential safety hazards of hydrogen leakage combustion blasting is greatly reduced; the method is applicable to the process of synthesizing the calcimimetics hydrochlorideintermediates.

Description

technical field [0001] The invention relates to a method for synthesizing a cinacalcet hydrochloride intermediate in a microchannel reactor, belonging to the field of drug synthesis in organic synthesis. Background technique [0002] Cinacalcet hydrochloride is a calcimimetic agent developed by the NPS company of the United States. It was approved for marketing by the FDA on March 8, 2004. The trade name is Sensipar, which is used for the treatment of secondary parathyroid function in patients with chronic kidney disease undergoing dialysis. Hypercalcemia, also used to treat hypercalcemia in patients with parathyroid cancer. Cinacalcet hydrochloride, a second-generation calcium receptor modulator, is used to treat hypercalcemia in patients with parathyroid carcinoma by activating hyperparathyroidism. Because its tablet is well absorbed in the human body, has high bioavailability, and is safe and well tolerated, it has a good market prospect. [0003] 3-(3-trifluoromethylph...

Claims

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Application Information

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IPC IPC(8): C07C57/58C07C51/36
CPCC07C51/36C07C57/58
Inventor 任吉秋杨昆李海涛
Owner HEILONGJIANG XINCHUANG BIOLOGICAL TECH DEV CO LTD
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