US 11,834,425 B2Granted

Full continuous-flow preparation method of vitamin B1

AssigneeFudan University

InventorsFener Chen, Meifen Jiang, Minjie Liu, Yingqi Xia, Weijian Li

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Abstract

A full continuous-flow preparation method of vitamin B1 includes: (S1) feeding 3-chloro-4-oxopentyl acetate, 2-methyl-4-amino-5-(aminomethyl) pyrimidine and carbon disulfide to a first continuous-flow reactor for addition; (S2) allowing the reaction mixture to flow into a first continuous filtration and reaction device to collect a filter cake; subjecting the filter cake and hydrochloric acid solution to cyclization; transporting the reaction mixture and an aqueous inorganic base solution to a micromixer and a second continuous-flow reactor for hydrolysis to obtain thiothiamine; (S3) transporting the thiothiamine to a third continuous-flow reactor with hydrogen peroxide for oxidation to obtain thiamine sulfate; and (S4) allowing the thiamine sulfate to enter a second continuous filtration and reaction device for filtration to collect a filter cake; and subjecting the filter cake to reaction with organic hydrochloric acid solution followed by filtration and drying to obtain vitamin B1.

Claims15

Dependent claims

A full continuous-flow preparation method of vitamin B1 using a continuous-flow reaction system, the continuous-flow reaction system comprising a first continuous-flow reactor, a first continuous filtration and reaction device, a micromixer, a second continuous-flow reactor, a third continuous-flow reactor, and a second continuous filtration and reaction device connected sequentially, and the full continuous-flow preparation method comprising:

(S1) feeding 3-chloro-4-oxopentyl acetate (3), 2-methyl-4-amino-5-(aminomethyl) pyrimidine (2) and carbon disulfide to the first continuous-flow reactor for addition reaction to obtain a first reaction mixture;
(S2) allowing the first reaction mixture to flow from the first continuous-flow reactor into the first continuous filtration and reaction device for filtration to collect a first filter cake;
subjecting the first filter cake and a hydrochloric acid solution to cyclization reaction to obtain a second reaction mixture;
and transporting the second reaction mixture together with an aqueous inorganic base solution to the micromixer and the second continuous-flow reactor for hydrolysis reaction to obtain thiothiamine (5);
(S3) transporting the thiothiamine and hydrogen peroxide to the third continuous-flow reactor for oxidation reaction to obtain thiamine sulfate (6);
and
(S4) allowing the thiamine sulfate to enter the second continuous filtration and reaction device for filtration to collect a second filter cake;
and subjecting the second filter cake to reaction with an organic hydrochloric acid solution followed by filtration and drying to obtain thiamine hydrochloride (1) as the vitamin B1;
as shown in the following reaction scheme:

6 more elements

Dependencies are inferred from the claim text.