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Novel crystal of pyrimidinedione compound hydrochloride and preparation method thereof

A kind of technology of compound and crystal form, applied in the field of pyrimidinedione compound hydrochloride

Inactive Publication Date: 2015-07-01
JIANGSU HANSOH PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are currently no reports on the crystal form

Method used

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  • Novel crystal of pyrimidinedione compound hydrochloride and preparation method thereof
  • Novel crystal of pyrimidinedione compound hydrochloride and preparation method thereof
  • Novel crystal of pyrimidinedione compound hydrochloride and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1: Preparation of Form I of Tipiracil Hydrochloride Using Dilute Hydrochloric Acid

[0021] Compound 1 (50g, 0.18mol) was added to purified water (250L), heated to 70°C to dissolve, then 25mL of concentrated hydrochloric acid was added dropwise, kept stirring and crystallized for 2h, then cooled down to room temperature for 2h. After filtering, the resulting solid was air-dried at 40°C until constant weight. The target product (42.3 g, white solid) was obtained with a yield of 84.6%.

Embodiment 2

[0022] Embodiment 2: Preparation of crystalline form I of Tipiracil hydrochloride using hydrochloric acid ethanol

[0023] Compound 1 (50g, 0.18mol) was added to purified water (250L), heated to 70°C to dissolve, then 25mL of concentrated hydrochloric acid was added dropwise, stirred and crystallized for 2h, 1000mL of ethanol was added, and the temperature was naturally cooled to room temperature for 2h. After filtering, the resulting solid was air-dried at 40°C until constant weight. The target product (46.5 g, white solid) was obtained with a yield of 93.0%.

experiment example 1

[0024] Experimental example 1: Influencing factor experiment

[0025] Instrument model: D8Advance Germany Bruker X-ray powder diffractometer;

[0026] Rays: monochromatic Cu-Kα rays

[0027] Scanning mode: θ / 2θ;

[0028] Scanning range: 2-40°;

[0029] Current: 40mA;

[0030] Voltage: 40kV.

[0031] The comparison of X-ray diffraction data is shown in Table 1.

[0032] Table 1 Statistics of influencing factors of crystal form I of the present invention

[0033]

[0034] It can be seen from the above experiments that the stability of the crystal form of the present invention is very good under various influencing factors, indicating that the crystal form is suitable for the development and application of new drugs.

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Abstract

The invention relates to a novel crystal of pyrimidinedione compound hydrochloride and a preparation method thereof. The invention discloses the novel crystal of 5-chloro-6-[(2-imino-1-pyrrolidyl)methyl]-2,4(1H, 3H)-pyrimidinedione hydrochloride shown in the formula I and the preparation method thereof. The novel crystal can produce X-ray diffraction peaks at diffraction angles 2 theta of 11.73 degrees, 13.03 degrees, 17.33 degrees, 17.97 degrees, 23.45 degrees, 27.23 degrees, 29.40 degrees and 32.85 degrees, has good stability and reappearance and is suitable for medicine development and application.

Description

technical field [0001] The present invention relates to pyrimidine diketone compound hydrochloride, especially Tipiracil hydrochloride 5-chloro-6-[(2-imino-1-pyrrolidine) methyl]-2,4(1H,3H)-pyrimidine Crystal form of diketone hydrochloride and preparation method thereof. Background technique [0002] TAS-102, developed by Taiho (a subsidiary of Otsuka Pharmaceutical Co., Ltd.), is a combination of the nucleoside analog trifluridine and the thymidine phosphorylase inhibitor (TIP) Tipracil hydrochloride (MUP-98156) , for the treatment of cancers including colorectal cancer. In February 2013, Taiho submitted an application for TAS-102 in Japan for the treatment of unresectable advanced recurrent colorectal cancer. In terms of market, this product is not yet on the market. [0003] According to statistics from the American Cancer Society, from 2005 to 2009, the incidence rate of colorectal cancer in the United States was 46.3 / 100,000 per year, and the incidence rate of the As...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D403/06
CPCC07B2200/13C07D403/06
Inventor 孙平李孝壁赵军军李赛
Owner JIANGSU HANSOH PHARMA CO LTD
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