A kind of preparation method of pramipexole hydrochloride
A technology of pramipexole hydrochloride and cyclohexanol, which is applied in the field of preparation of pramipexole hydrochloride, can solve the problems of high environmental pollution, difficulty in industrial production of pramipexole hydrochloride, low yield, etc. Prospects and industrialization should be valuable, and the effect of cheap and easy-to-obtain raw materials
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Embodiment 1
[0035] The preparation method of a kind of pramipexole hydrochloride proposed by the present invention comprises the following steps: firstly protect the amino group of p-aminocyclohexanol through propionyl chloride condensation to obtain p-propionylamino cyclohexanol, and then obtain p-propionylamino cyclohexanol through catalytic oxidation Hexanone, followed by oxidative bromination and Hantzsch condensation to obtain 2-amino-6-propionylamino-4,5,6,7-tetrahydrobenzothiazole, and then reduced by diisobutylaluminum hydride to obtain 2-amino- 6-propylamino-4,5,6,7-tetrahydrobenzothiazole, and then use L-(+)-tartaric acid as a resolving agent to carry out a resolution reaction, and finally form a salt to obtain pramipexole hydrochloride.
Embodiment 2
[0037] The preparation method of a kind of pramipexole hydrochloride proposed by the present invention comprises the following steps: first, p-aminocyclohexanol is condensed with propionyl chloride to protect the amino group to obtain p-propionylaminocyclohexanol, wherein, propionyl chloride and p-aminocyclohexanol The molar ratio between them is 1:1, and the reaction temperature is -30°C; Then, p-propionylaminocyclohexanone is obtained through catalytic oxidation, wherein, in the catalytic oxidation process, TCCA is selected as the oxidant, TEMPO and NaBr are selected as the catalyst, and Dichloromethane is used as a solvent, and the molar ratio between propionylaminocyclohexanol, TCCA, TEMPO, and NaBr is 2:1:0.02:0.2, and the reaction temperature is -10°C; then oxidative bromination and Hantzsch condensation Pot method to obtain 2-amino-6-propionylamino-4,5,6,7-tetrahydrobenzothiazole, wherein, in the oxidative bromination process, the oxidative bromination reagent is H 2 o ...
Embodiment 3
[0039] The preparation method of a kind of pramipexole hydrochloride proposed by the present invention comprises the following steps: first, p-aminocyclohexanol is condensed with propionyl chloride to protect the amino group to obtain p-propionylaminocyclohexanol, wherein, propionyl chloride and p-aminocyclohexanol The molar ratio between is 1.5:1, and reaction temperature is 30 ℃; Then obtain p-propionylaminocyclohexanone through catalytic oxidation, wherein, in the catalytic oxidation process, select TCCA as oxidant for use, select TEMPO, NaBr as catalyst for use, select two Chloromethane is used as a solvent, and the molar ratio between propionylaminocyclohexanol, TCCA, TEMPO, and NaBr is 1:0.5:0.01:0.1, and the reaction temperature is 40°C; and then oxidative bromination and Hantzsch condensation one-pot method Obtain 2-amino-6-propionylamino-4,5,6,7-tetrahydrobenzothiazole, wherein, in the oxidative bromination process, the oxidative bromination reagent is H 2 o 2 / HBr; a...
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