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Crystalline form of N-methyl-N-((3R,4R)-4-methyl-1-benzyl-3-piperidyl)-7H-pyrrolo[2,3-D]pyrimidine-4-amine

A -4-, 3-D technology, applied in the field of crystallization and preparation of intermediates, can solve the problems of unfavorable industrialization and commercial sales, poor stability, and low purity, and achieve simple and reliable preparation methods, good stability, and high purity high effect

Inactive Publication Date: 2016-02-03
SHANDONG ACADEMY OF PHARMACEUTICAL SCIENCES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The technical problem to be solved by the present invention is to provide a new crystallization of a tofacitinib intermediate and a preparation method thereof, which overcomes the poor stability of the tofacitinib intermediate compound 1 in the existing technology, is not easy to preserve, and has low purity , Defects that are not conducive to industrialization and commercial sales

Method used

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  • Crystalline form of N-methyl-N-((3R,4R)-4-methyl-1-benzyl-3-piperidyl)-7H-pyrrolo[2,3-D]pyrimidine-4-amine
  • Crystalline form of N-methyl-N-((3R,4R)-4-methyl-1-benzyl-3-piperidyl)-7H-pyrrolo[2,3-D]pyrimidine-4-amine
  • Crystalline form of N-methyl-N-((3R,4R)-4-methyl-1-benzyl-3-piperidyl)-7H-pyrrolo[2,3-D]pyrimidine-4-amine

Examples

Experimental program
Comparison scheme
Effect test

example 2

[0043] Refer to Example 2 (Refer to CN200680027901.3 Example 8) Preparation of compound 4:

[0044] Add 2kg compounds to the reaction kettle 6, water and 2kg compound 5, mix and add 2.7kg of potassium carbonate, increase the temperature to return, the reaction is 10 hours, TLC monitoring reaction completely cools to 50 ° C, add 2L acetylene, stir at 50 ° C 1 1In the hour, stir to 20 ° C for 3 hours, filter, wash and dry, and get 4 about 3.2kg.

example 3

[0045] Refer to Example 3 (Refer to CN200680027901.3 Example 9) Preparation of compound 1:

[0046] Stir at 20 ° C for 1 hour, centrifugal, dry at 50 ° C to obtain white solids, that is, a compound of 1 is about 1.7kg.(HPLC purity 88.92%).The sampling of X-ray diffraction test analysis is a non-fixed powder.

Embodiment 1

[0047] Example 1 compound 1 Crystal form Preparation:

[0048] Crystallization Compound 1, 85%of the income, HPLC purity 99.84%.

[0049] The Crystal DSC detection graph has a hot peak at 149.7 ° C; after the X-ray diffraction test analysis, the test conditions are as follows: Panalyticalx'PERTPRO powder X-ray diffraction meter is determined, and CUKA40KV40MA is the light source, the step length is 0.02 °, and the scanning speed:8 ° / min, scanning range: 3 ° ~ 80 °, room temperature.The results of powder X-ray diffraction analysis are shown in Table 1.

[0050]Table 1 Example 1 Powder X-ray diffraction data of Chinese compound 1

[0051] Peak number number 2 θ angle (± 0.2 °) Relative Strength% 1 8.6° 12.0 2 13.9° 20.8 3 15.8° 29.1 4 17.2° 100.0 5 18.4° 14.0 6 25.9° 39.8

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Abstract

The invention discloses a Tofacitinib midbody, i.e. a new crystalline form of N-methyl-N-((3R,4R)-4-methyl-1-benzyl-3-piperidyl)-7H-pyrrolo[2,3-D]pyrimidine-4-amine, a preparation method thereof, and a method of preparing Tofacitinib by using a midbody of the crystal form. The midbody of the crystal form has the advantages of high purity, good stability, simple preparation, easy production and sales.

Description

Technical field [0001] The invention involves the crystallization, preparation method of a drug intermediate, and its purpose in preparing the Telobitinib, which involves the crystallization and preparation methods of the intermediate of a Tasitinib. Background technique Background technique [0002] Tofacitinib is a new type of oral JAK pathogenesis developed by Pfizer.Unlike most other RA therapy drugs, which are mainly based on extracellular targets, the Toffetu is the core part of the cytokine network with intracellular signal transitional pathways.Tofacitinib's inhibitory intensity of Jak3 is 5 to 100 times the Jak1 and Jak2.Toffubo is the first-in-in-classdrug for developing rheumatoid arthritis therapy. FDA approved the JAK inhibitor TOFACITINIB on November 6, 2012 for the treatment of adult activity during the treatment of adults and alima butterfliesPatients with poor response (MTX) patients with poor reactions.FDA said that patients with medium to severe rheumatoid a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/04
CPCC07D487/04C07B2200/13
Inventor 毋立华张治云刘荣磊李帅刘亚芳张利剑郑德强段崇刚
Owner SHANDONG ACADEMY OF PHARMACEUTICAL SCIENCES
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