N-[(3R,4R)-1-benzyl-4-methylpiperidine-3-yl]-N-methyl-7H-pyrrolo[2,3-d] pyrimidine-4-amine crystal

A technology of methylpiperidine and methylaminopiperidine dihydrochloride, which is applied in the most critical intermediate field of tofacitinib citrate, can solve the problems affecting the quality of the final product tofacitinib citrate, etc. Achieve the effect of major technical advantages and research value
CN105153166AInactive Publication Date: 2015-12-16HUBEI LIYI PHARM TECH CO LTD +1
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
HUBEI LIYI PHARM TECH CO LTD
Publication Date
2015-12-16
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention discloses an N-[(3R,4R)-1-benzyl-4-methylpiperidine-3-yl]-N-methyl-7H-pyrrolo[2,3-d] pyrimidine-4-amine crystal and a preparation method thereof. The method comprises steps as follows: firstly, 4-chloro-7-(p-tolylsulfonyl) pyrrolo [2,3-d] pyrimidine, 1-benzyl-4-methyl-3-aminomethyl dihydrochloride, potassium carbonate and water are added to a reaction vessel sequentially, heated and subjected to thermal insulation, and white solids are obtained; the white solids, sodium hydroxide and n-butyl alcohol are added to the reaction vessel sequentially, an obtained organic phase is washed with water, then anhydrous magnesium sulfate is added to the organic phase for dehydration, and a dichloromethane extracting solution is obtained; finally, eluting and curing are performed, and the crystal is obtained. The purity of the crystal is higher than 99.9%. According to a final product tofacitinib citrate synthesized with the intermediate, related substances are controlled to be lower than 0.1%, and the preparation of the crystal has great technical advantage and research value.
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Description

technical field

[0001] The present invention relates to the most critical intermediate of tofacitinib citrate, specifically a kind of N-[(3R,4R)-1-benzyl-4-methylpiperidin-3-yl]-N-methyl Cyl-7H-pyrrolo[2,3-d]pyrimidin-4-amine (hydrolyzate for short) crystal and preparation method thereof. Background technique

[0002] The structural formula of N-[(3R,4R)-1-benzyl-4-methylpiperidin-3-yl]-N-methyl-7H-pyrrolo[2,3-d]pyrimidin-4-amine is as follows:

[0003]

[0004] The U.S. Food and Drug Administration approved Pfizer's Xeljanz (tofacitinib, tofacitinib citrate) in November 2012 for moderately to severely active rheumatoid arthritis ( RA) for the treatment of adult patients.

[0005] Tofacitinib citrate is used for the treatment of active rheumatoid arthritis (RA), and the patient group is moderate to severe adult patients who have insufficient response or intolerance to methotrexate treatment. RA is an autoimmune disease in which the immune system mistakenly attacks, cau...

Claims

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