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Method for purifying bendamustine hydrochloride

A technology of bendamustine hydrochloride and a purification method is applied in the field of purification of bendamustine hydrochloride to achieve the effects of good product quality, short cycle and simple process

Active Publication Date: 2012-05-30
浙江凯普化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But bendamustine hydrochloride with higher purity (especially HP1 content less than 0.1%) is difficult to obtain by existing methods

Method used

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  • Method for purifying bendamustine hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] 10 grams of bendamustine hydrochloride crude product (containing HP1 1.8%) was placed in a flask, and 50 milliliters of 0.01N hydrochloric acid was added. Rapidly heated until the solution became clear, then placed in ice water and cooled to 0°C for recrystallization. Filter, filter cake is dried 24 hours in high vacuum (<1 mm Hg), obtain 8.6 grams of high-purity bendamustine hydrochloride (content (HPLC): 99.9%; HP1: 0.06%, other impurity: 0.08%, Water content: 0.9%).

[0014] 1 H-NMR (DMSO-d6, 400MHz): δ7.70(d, 1H), 7.07(d, 1H), 6.88(s, 1H), 3.87(s, 3H), 3.74(m, 8H), 3.14( t, 2H), 2.38(t, 2H), 1.99(m, 2H). Elemental analysis C 16 h 22 Cl 3 N 3 o 2 Calculated (%): C, 48.68; H, 5.62; N, 10.65; Cl, ​​26.95; found (%): C, 47.96; H, 5.64; N, 10.43; Cl, ​​26.00.

Embodiment 2

[0016] 10 grams of crude bendamustine hydrochloride (containing 1.8% HP1) was placed in a flask, and 50 milliliters of 0.1N hydrochloric acid was added. Rapidly heated until the solution became clear, then placed in ice water and cooled to room temperature for recrystallization. Filter, filter cake is dried 24 hours in high vacuum (<1 mm Hg), obtain 8.1 grams of high-purity bendamustine hydrochloride (content (HPLC): 99.9%; HP1: 0.07%, other impurity: 0.06%, Water content: 0.7%).

Embodiment 3

[0018] 10 grams of bendamustine hydrochloride crude product (containing HP1 1.8%) was placed in a flask, and 50 milliliters of 1N hydrochloric acid was added. Rapidly heated until the solution became clear, then placed in ice water and cooled to 35°C for recrystallization. Filter, filter cake is dried 24 hours in high vacuum (<1 mm Hg), obtain 7.2 grams of high-purity bendamustine hydrochloride (content (HPLC): 99.9%; HP1: 0.05%, other impurity: 0.05%, Water content: 0.9%).

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Abstract

The invention discloses a method for purifying bendamustine hydrochloride, which comprises the following steps of: dissolving a bendamustine hydrochloride crude product into hydrochloric acid solution for recrystallization, and performing filtration to obtain pure bendamustine hydrochloride. The method belongs to the fields of organic chemistry and medicinal chemistry, and has the advantages of simple process, short cycle, high yield, high quality of product, suitability for industrial production and the like.

Description

technical field [0001] The invention relates to a method for purifying bendamustine hydrochloride, belonging to the fields of organic chemistry and medicinal chemistry. Background technique [0002] Bendamustine (as shown in structural formula I) is a bifunctional alkylating agent used for the treatment of chronic lymphocytic leukemia and non-Hodgkin's lymphoma (NHL), which can significantly reduce the recurrence rate and mortality. In 1963, Ozegowski and Krebs synthesized bendamustine. Until 1990, it only applied to East Germany. East German studies found that bendamustine is suitable for the treatment of chronic lymphocytic leukemia, Hodgkin's disease, non-Hodgkin's lymphoma, multiple myeloma and lung cancer. In March 2008, the US FDA approved Bendamustine Hydrochloride (Bendamustine Hydrochloride, trade name: Treanda) of Cephalon Company for the treatment of chronic lymphocytic leukemia (CLL). Bendamustine is the first drug approved in the United States for patients wi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D235/16
Inventor 谭翔晖黄建周忱
Owner 浙江凯普化工有限公司
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