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Novel crystal form of Tipracil hydrochloride and preparation method thereof

A technology of crystal form and hydrochloric acid, applied in the field of new crystal form of Tipracil hydrochloride and its preparation

Pending Publication Date: 2015-09-30
JIANGSU HANSOH PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

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Method used

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  • Novel crystal form of Tipracil hydrochloride and preparation method thereof
  • Novel crystal form of Tipracil hydrochloride and preparation method thereof
  • Novel crystal form of Tipracil hydrochloride and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1 uses dilute hydrochloric acid to prepare the crystal form II of Tipiracil hydrochloride

[0028] Add compound 1 (50g, 0.18mol) into purified water (500ml), stir at 20°C until dissolved, then add 50ml of concentrated hydrochloric acid dropwise, during the dropwise addition, crystals gradually precipitate out, and after dropping, continue stirring at this temperature Crystal 2h. After filtering, the resulting solid was air-dried at 40°C until constant weight. The target product (41.5 g, white solid) was obtained with a yield of 83%.

[0029] figure 2 is the X-ray diffraction pattern of the crystal form II of the sample prepared in Example 1.

Embodiment 2

[0030] Embodiment 2 uses acetone hydrochloride to prepare the crystal form II of Tipiracil hydrochloride

[0031] Compound 1 (50 g, 0.18 mol) was added into purified water (500 ml), stirred at 20° C. until dissolved, and a mixed solvent of 25 ml of hydrochloric acid and 2 L of acetone was added to the clear liquid. After continuing to stir at this temperature for about 20 minutes, crystals gradually precipitated out, and continued to stir and crystallize for 2 hours. After filtering, the resulting solid was air-dried at 40°C until constant weight. The target product (43.5 g, white solid) was obtained with a yield of 87%.

[0032] image 3 is the X-ray diffraction pattern of the crystal form II of the sample prepared in Example 2.

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Abstract

The invention discloses a new crystal form of Tipracil hydrochloride and a preparation method thereof. Particularly, the invention relates to a crystal form of Tipracil hydrochloride shown in the formula (1), namely 5-chloro-6-[(2-imino-pyrrolidine) methyl]-2,4(1H,3H)-pyrimidinedione hydrochloride, and a preparation method of the new crystal form of Tipracil hydrochloride. The crystal form is stable and easily prepared and meets the application requirement of medicine preparations. The formula (1) is shown in the specification.

Description

technical field [0001] The present invention relates to the crystal form of Tipiracil hydrochloride 5-chloro-6-[(2-imino-1-pyrrolidinyl)methyl]-2,4(1H,3H)-pyrimidinedione hydrochloride and its preparation method. Background technique [0002] Tipiracil hydrochloride (Tipiracil hydrochloride), TAS-102 developed by Taiho (a subsidiary of Otsuka Pharmaceutical in Japan), is a nucleoside analog trifluridine and a thymidine phosphorylase inhibitor (TIP) tipracilhydrochloride (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 Asian population was about 40 / 100,0...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D403/06
Inventor 李赛孙平王俊亮余雷
Owner JIANGSU HANSOH PHARMA CO LTD
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