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Process for preparing argatroban hydrate

A technology of argatroban and hydrate, which is applied in the field of preparation of argatroban hydrate, can solve problems such as nonconformity, low yield, and large ratio change, and achieve mild operating conditions, high yield, and high product quality. high effect

Active Publication Date: 2008-10-22
TIANJIN WEIJIE TECH
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  • Application Information

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Problems solved by technology

[0011] The method reported in the above literature is recrystallized with 15% ethanol, and the ratio of R and S varies greatly, which does not meet the range of medical R:S=63~67:37~33, and cannot remove other organic impurities well, so it is difficult to guarantee Product quality, lower yields, sometimes not guaranteed full hydration

Method used

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  • Process for preparing argatroban hydrate
  • Process for preparing argatroban hydrate
  • Process for preparing argatroban hydrate

Examples

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Embodiment 1

[0021] Embodiment 1. 65g Argatroban (R: S=65: 35) solid is added in 4200ml distilled water, slowly warming up to reflux, after all the solid dissolves, naturally cool to room temperature, white crystals are separated out, filter. Wash twice with water and dry within 100°C to obtain Argatroban monohydrate Add 65g of Argatroban (R:S=65:35) to 4200ml of distilled water, slowly heat up to reflux, after all the solids are dissolved, naturally cool to room temperature, and white Crystallized, filtered. Wash twice with water and dry within 100°C to obtain 59 g of Argatroban monohydrate. Yield 87.3%. 21(R):21(S)=64.5:34.5 (HPLC method), water content 3.55% (Karl Fischer method).

[0022] Elemental analysis:

[0023] Experimental value: S: 5.95% N: 15.05% H: 7.35%

[0024] Calculated (C23H38N6O6S): S: 6.08% N: 15.96% H: 7.27%

Embodiment 2

[0025] Example 2. 50 grams of Argatroban (R:S=65:35) was added to 4000ml of distilled water, the temperature was raised to 90° C., the reaction was stirred for two hours, then naturally cooled to room temperature, white crystals were precipitated, and filtered. Wash twice with water and dry within 100°C to obtain 46.8 g of Argatroban monohydrate with a yield of 90.4%. 21(R):21(S)=64.8:35.2 (HPLC method), water content 3.34% (Karl Fischer method).

[0026] Elemental analysis:

[0027] Experimental value: S: 5.87% N: 15.23% H: 7.05%

[0028] Calculated (C23H38N6O6S): S: 6.08% N: 15.96% H: 7.27%

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Abstract

The invention discloses a preparing method of Argatroban hydrate, which comprises the following steps: refluxing Argatroban and water for 0.5-1.0h; dissolving; cooling to indoor temperature; evolving white crystal; filtering; washing twice; drying to obtain medical Argatroban hydrate. The invention guarantees the constant rate of R and S without other organic impurity, which improves hydrating receiving rate between 90% and 95%.

Description

technical field [0001] The invention relates to a preparation method of argatroban hydrate. technical background: [0002] In 1978, the antithrombin activity of argatroban (Argatroban) hydrate was first reported by S.Okamoto of Japan Mitsubishi Chemical Company [US 4 101 653]. During the following 20 years, many researchers conducted in-depth research on the biological activity of Argatroban and its value as medicine. In 1981, S.Okamoto compared heparin in animals [Okamoto, S.et al., Biochem.Biophys.Res.Commun.101, 440 (1981)]; T.Kumoto et al. Reported [Kumada, T.et al., Thromb.Res.24, 285 (1981)]; In 1984, R.Kumato carried out clinical hemodialysis evaluation [Kikumoto, R.et al., Biochemistry 23, 85 (1984) ]; In 1986, the author reported that Argatroban inhibited thrombin activity in mammals, which can be used as a treatment and prevention agent for thrombosis and platelet aggregation inhibitor. Argatroban monohydrate can be used as a selective antithrombotic agent to tr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D401/12C07D215/00C07D211/00
Inventor 宋洪海
Owner TIANJIN WEIJIE TECH
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