Preparation method and preparation of large crystalline form of vorinostat I

A vorinostat, large-grain technology, which is applied in the field of preparation and preparation of vorinostat I crystal-form large-grain, can solve problems such as cumbersome locks, and achieve the effect of good dissolution effect and great commercial application value

Active Publication Date: 2016-08-03
杭州容立医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that it is too cumbersome

Method used

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  • Preparation method and preparation of large crystalline form of vorinostat I
  • Preparation method and preparation of large crystalline form of vorinostat I
  • Preparation method and preparation of large crystalline form of vorinostat I

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Methanol / water crystallization method

[0027] Heat 1635ml of methanol / water (6 / 1) and 218g of vorinostat to reflux, stir to dissolve, add 1.0g of activated carbon, filter while hot, add 469ml of water to the filtrate, heat up to 70°C to dissolve, cool to 63°C, add a small amount of vorinostat I crystal seed crystals, keep warm at 60-63°C for 3 hours, slowly precipitate solids, then cool down 1°C per hour until the temperature drops to 50°C, then cool down to below 30°C, filter, filter cake Wash with 150ml of water. The solid powder was obtained and dried to obtain 196 grams of vorinostat I crystal form.

Embodiment 2

[0029] Methanol / water crystallization method

[0030] Heat 1635ml of methanol / water (6 / 1) and 218g of vorinostat to reflux, stir to dissolve, add 1.0g of activated carbon, filter while hot, add 469ml of water to the filtrate, heat up to 70°C to dissolve, cool to 63°C, add a small amount of vorinostat I crystalline seed crystals, keep warm for 3 hours, slowly precipitate solids, then lower the temperature by 0.2°C per hour until the temperature drops below 30°C, filter, and wash the filter cake with 150ml of water. The solid powder was obtained and dried to obtain 196 grams of vorinostat I crystal form.

Embodiment 3

[0032] Methanol / water crystallization method

[0033] Heat 1635ml of methanol / water (6 / 1) and 218g of vorinostat to reflux, stir to dissolve, add 1.0g of activated carbon, filter while hot, add 469ml of water to the filtrate, heat up to 70°C to dissolve, cool to 63°C, add a small amount of vorinostat I crystalline seed crystals, keep warm for 3 hours, and slowly precipitate solids, then lower the temperature by 0.5°C per hour until the temperature drops below 0°C, filter, and wash the filter cake with 150ml of water. The solid powder was obtained and dried to obtain 199 g of vorinostat I crystal form.

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Abstract

The invention provides a method for preparing large crystalline vorinostat I crystal grains for treating skin T-cell lymphoma and a preparation made of vorinostat obtained therefrom. The above preparation method can crystallize in place at one time, is simple and effective, is suitable for large-scale industrial production, and has great commercial application value. The obtained preparation has good dissolution effect.

Description

technical field [0001] The invention relates to a method for preparing large crystal grains of vorinostat (vorinostat) I, a drug for treating skin T-cell lymphoma, and a preparation thereof. technical background [0002] Vorinostat (formula I) is a protein deacetylase (HDAC) inhibitor. The drug has been approved by the US FDA as a rare disease drug in 2006 for the treatment of cutaneous T-cell lymphoma (cutaneous T-cell lymphoma, CTCL), when the disease continues to worsen or relapses during or after treatment with other drugs. [0003] [0004] The synthesis method of vorinostat has been reported in WO9307148, JMedChem1995, 38(8): 1411, OrgPrepProcedInt2001, 33(4): 391, CN200680000867.0 and other documents. Vorinostat has polymorphism, and the crystalline form of the vorinostat bulk drug listed by foreign original research companies is I crystalline form, and the DSC figure of I crystalline form (see figure 1 ), the analysis is shown in Table 1, and its X-diffraction p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C259/06A61K31/167A61K9/48A61P35/00
Inventor 任建强施水萍胡雅芳邵秀芬王万青钟万德
Owner 杭州容立医药科技有限公司
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