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Preparation of bromocriptine mesylate

A technology of bromocriptine mesylate and methanesulfonic acid, applied in the field of chemical preparation, can solve the problems of many impurities and difficult to remove, and achieve the effects of high purity, easy recovery and high yield

Active Publication Date: 2022-08-05
TIANJIN PRECEDE MEDICAL TRADE
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0030] The present inventors found that the preparation of bromocriptine mesylate disclosed in the prior art, the final step of bromocriptine and methanesulfonic acid reaction to obtain the reaction of 2-bromo-alpha-ergocriptine mesylate, the product after salt formation There are many impurities in the medium, because the solvents used in the salt-forming reaction mainly include dichloromethane, acetone, butanone, etc. These solvents are conducive to the dissolution of impurities in the reaction product of the previous step. The relevant impurities include: impurities A-E, wherein impurity B is the raw material α -Ergocriptine, the impurity content is high, and it is soluble in the reaction solvent, and it is difficult to remove it by simple recrystallization method, so after the salt is formed, complex purification treatment is required to ensure the impurity content is qualified

Method used

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  • Preparation of bromocriptine mesylate
  • Preparation of bromocriptine mesylate
  • Preparation of bromocriptine mesylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Dissolve 6.54g (0.01 mol) of bromocriptine in 100 ml of methanol, and add 10 ml of a newly prepared aqueous methanesulfonic acid solution (containing 1.44 g (0.015 mol) of methanesulfonic acid) dropwise within 5 minutes under stirring. After the dropwise addition, Continue stirring for 30 minutes, cool to 4° C., stand for 2 hours, filter to obtain solid, recrystallize the solid once with 75 ml of 95% ethanol, filter and dry to obtain 7.2 g of bromocriptine mesylate with a yield of 95.5%. HPLC detection showed that the purity of bromocriptine mesylate was 99.1%, and there was almost no α-ergocriptine peak of bromocriptine impurity.

Embodiment 2

[0068] 6.54g (0.01 mol) of bromocriptine was dissolved in 100 ml of methanol, and 20 ml of a newly prepared methanesulfonic acid aqueous solution (containing 1.20 g (0.0125 mol) of methanesulfonic acid) was added dropwise within 10 minutes of stirring. After the dropwise addition, Continue to stir for 20 minutes, cool to 4°C, stand for 2 hours, filter to obtain a solid, recrystallize the solid once with 75 ml of 95% ethanol, filter and dry to obtain 6.85 g of bromocriptine mesylate, yield 91.2%, HPLC detection, methanesulfonic acid The purity of bromocriptine sulfonate is 99.0%, and there is impurity α-ergocriptine peak, and the content is 0.006%.

Embodiment 3

[0070] Dissolve 6.54g (0.01mol) of bromocriptine in 100ml of methanol, add 20ml of newly prepared methanesulfonic acid aqueous solution (containing 1.15g (0.012mol) of methanesulfonic acid) dropwise within 20 minutes of stirring, and finish the dropwise addition Then, continue stirring for 30 minutes, stand at room temperature for 2 hours, filter to obtain a solid, recrystallize the solid once with 75 ml of 95% ethanol, filter and dry to obtain 7.01 g of bromocriptine mesylate, yield 93.4%, HPLC detection, methanesulfonic acid The purity of bromocriptine acid is 98.9%, and there is impurity α-ergocriptine peak, and the content is 0.08%.

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Abstract

The present invention relates to a preparation method of bromocriptine mesylate. The method comprises the following steps: dissolving bromocriptine in methanol, and adding dropwise newly prepared methanesulfonic acid with a dosage of 1.1-1.5 times the molar amount of bromocriptine under stirring. The acid aqueous solution, after the dropwise addition, continued to stir for 10-40 minutes, cooled to 0° C. to room temperature, and filtered to obtain a solid. The solid was recrystallized once with ethanol, and filtered and dried to obtain bromocriptine mesylate.

Description

Technical field: [0001] The invention relates to a preparation method of a chemical drug, in particular to a preparation method of bromocriptine mesylate. Background technique: [0002] Bromocriptine, also known as: bromocriptine or bromocriptine, is a drug developed by Novartis, Italy. The structure of bromocriptine is as follows: [0003] [0004] The mesylate salt of bromocriptine (launched in 1976) is clinically used to treat the following diseases: [0005] 1. Endocrine system diseases: prolactin-dependent menstrual cycle disorders and infertility (with hyper or normoprolactinemia), amenorrhea (with or without lactation), oligomenorrhea, luteal insufficiency, and drug-induced Hyperprolactinism (antipsychotics and high blood pressure medication). [0006] 2. Non-prolactin-dependent infertility: polycystic ovary syndrome, combined with anti-estrogens (such as: clodophenamine) to treat anovulation. [0007] 3. Hyperprolactinoma: Conservative treatment of small pituit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D519/02C07C303/32C07C303/44C07C309/04
CPCC07D519/02C07C303/32C07C303/44C07C309/04
Inventor 杨兵
Owner TIANJIN PRECEDE MEDICAL TRADE
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