A kind of method that microchannel reactor synthesizes crizotinib intermediate
A microchannel reactor, a technology for synthesizing crizotinib, applied in chemical instruments and methods, chemical/physical/physical-chemical reactors, organic chemistry, etc. Chlorine side reaction and other problems, to achieve the effect of stable online production and post-treatment, production economic guarantee, and production cost reduction
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Embodiment 1
[0039] This embodiment provides a method for the synthesis of crizotinib intermediates in a microchannel reactor, such as figure 1 with figure 2 As shown, the microchannel reactor used includes a preheating module, a reaction module group and a cooling module, wherein: the preheating module is connected in series with the reaction module group, the cooling module is connected in series with the reaction module group, and the reaction module group includes a unit reaction module Or be formed by the serial combination of more than two unit reaction modules; The synthetic method of 2-amino-5-chlorobenzophenone comprises the following steps:
[0040] 1) Weigh 200g of raw material 3-(1-(2,6-dichloro-3-fluorophenyl)ethoxy)-2-nitropyridine, then add it to the mixture of 2L methanol and 2L ethyl acetate In the liquid, after stirring and dissolving, add 10g of Pt / C catalyst with a mass content of 5% and fully stir and mix to form material I, which is transported to the preheating mo...
Embodiment 2
[0043] This embodiment provides a method for the synthesis of crizotinib intermediates in a microchannel reactor, such as figure 1 with figure 2 As shown, the microchannel reactor used includes a preheating module, a reaction module group and a cooling module, wherein: the preheating module is connected in series with the reaction module group, the cooling module is connected in series with the reaction module group, and the reaction module group includes a unit reaction module Or be formed by the serial combination of more than two unit reaction modules; The synthetic method of 2-amino-5-chlorobenzophenone comprises the following steps:
[0044] 1) Weigh 250g of the raw material 3-(1-(2,6-dichloro-3-fluorophenyl)ethoxy)-2-nitropyridine, and add it to a mixture of 2.5L methanol and 2.5L tetrahydrofuran In, after stirring and dissolving, add 12g of Pt / C catalyst with a mass content of 6% to fully stir and mix to form material I, and material I is transported to the preheatin...
Embodiment 3
[0047] This embodiment provides a method for the synthesis of crizotinib intermediates in a microchannel reactor, such as figure 1 with figure 2 As shown, the microchannel reactor used includes a preheating module, a reaction module group and a cooling module, wherein: the preheating module is connected in series with the reaction module group, the cooling module is connected in series with the reaction module group, and the reaction module group includes a unit reaction module Or be formed by the serial combination of more than two unit reaction modules; The synthetic method of 2-amino-5-chlorobenzophenone comprises the following steps:
[0048] 1) Weigh 180g of the raw material 3-(1-(2,6-dichloro-3-fluorophenyl)ethoxy)-2-nitropyridine, and add it to a mixture of 1.8L of ethanol and 1.8L of acetonitrile In, after stirring and dissolving, add 15g of Pd / C catalyst with a mass content of 8% and fully stir and mix to form material I. Material I is transported to the preheating...
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