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
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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, and the ...
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 flow ...
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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