Preparation method for azacitidine crystal form I

A technology for azacitidine crystals and azacitidine crude products, which is applied in the field of preparation of azacitidine crystal form I, can solve the problems of unsatisfactory impurity control and high solvent residue, and achieve good impurity removal effect and high purity. Effect

Active Publication Date: 2018-12-04
NANJING SHUNXIN PHARM CO LTD OF CHIATAI TIANQING PHARM GRP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, there are still some problems in the improved method of US2004186284, such as unsatisfactory impurity control, high solvent residue

Method used

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  • Preparation method for azacitidine crystal form I
  • Preparation method for azacitidine crystal form I
  • Preparation method for azacitidine crystal form I

Examples

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Comparison scheme
Effect test

Embodiment 1

[0046] Example 1: Preparation method of azacitidine crystal form I

[0047] 10.0g crude azacitidine was added to 40ml dimethyl sulfoxide, dissolved at 50-60°C, 176ml purified water was added, then 275ml absolute ethanol was added, and crystallization was stirred at 0-5°C for 1h. After filtration, the obtained solid was added to 200ml of absolute ethanol, stirred at room temperature for 2h, filtered, and dried to obtain 8.8g of azacitidine crystal form I.

Embodiment 2

[0048] Example 2: Preparation method of azacitidine crystal form I

[0049] Add 5.0g of crude azacitidine to 20ml of dimethyl sulfoxide, dissolve it at 50-60°C, add 80ml of purified water, then add 100ml of absolute ethanol, and stir and crystallize at 0-5°C for 2h. After filtration, the obtained solid was added to 30 ml of absolute ethanol, stirred at room temperature for 0.5 h, filtered, and dried to obtain 4.0 g of azacitidine crystal form I.

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Abstract

The invention provides a preparation method for azacitidine crystal form I. The preparation method is to put an azacytidine crude product into a mixed solvent including three solvents which are a polar non-protonic solvent, C2-C4 alcohol and water to perform recrystallization, so that the azacitidine crystal form I which has high purity, low impurity content and nearly no solvent residue can be obtained.

Description

Technical field [0001] The invention belongs to the field of medicinal chemistry, and relates to a preparation method of azacitidine crystal form I, and specifically relates to the preparation of azacitidine crystal form I using a mixed solvent including three types of solvents. Background technique [0002] Azacitidine (azacitidine) is a cytosine nucleoside analogue. As a nucleoside metabolism inhibitor, it was marketed in the United States in 2004 under the trade name Vidaza. It is used to treat all FAB types of myelodysplastic syndromes. Including refractory anemia, refractory anemia with ring sideroblasts, refractory anemia with increased blasts, chronic myelomonocytic leukemia, refractory anemia with increased blasts and transformation. [0003] At present, the synthesis of azacitidine mainly adopts the following methods, which have been published in many documents. [0004] [0005] At present, the crystal form of azacitidine has also been published in many documents. Among t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H19/12C07H1/06
CPCC07H1/06C07H19/12C07B2200/13
Inventor 郭猛余孔强宋开镇邵磊夏春光张喜全
Owner NANJING SHUNXIN PHARM CO LTD OF CHIATAI TIANQING PHARM GRP
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