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Improved method of preparing secnidazole

A kind of technology of other butnidazole and nitro group is applied in the field of preparing other butnidazole-2-methyl-5-nitro-1H-imidazole), can solve problems such as low yield, and achieve the effect of less consumption

Inactive Publication Date: 2006-10-11
UNICHEM LAB LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] a) The yield is low, only 3.62%

Method used

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  • Improved method of preparing secnidazole
  • Improved method of preparing secnidazole
  • Improved method of preparing secnidazole

Examples

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Embodiment 1

[0030] 2-Dimethyl-5-nitro-1H-imidazole-1-ethanol (i.e. another butinidazole, also known as 1-(2-hydroxypropyl)-2-methyl-5-nitro-1H-imidazole ) preparation method

[0031] In a 5-liter four-necked flask with a cooling device and a dropping funnel with a jacket, add 1600ml of anhydrous ethyl acetate, cool to 0-5 degrees Celsius under stirring, and slowly add 400g (3.0mol) of anhydrous chlorinated Aluminum, keep the temperature between 0-5 degrees Celsius. To the resulting clear solution was added 200 g (1.5748 mol) of 2-methyl-5-nitro-imidazole. Observe for a thick slurry. Keep the temperature at 0-5 degrees Celsius, add 160 g (2.75 mol) of propylene oxide dropwise, and control the dropping rate at about 1 hour. The reactant was continuously stirred for 3 hours at a temperature of 0-5 degrees Celsius, then poured into diluted hydrochloric acid, and stirred for 15 minutes. The reaction solution was filtered to remove unreacted 2-methyl-5-nitro-imidazole. Dry at -80°C for 24 ...

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Abstract

The present invention discloses an improved method for the preparation of butynidazole (i.e. 2-dimethyl-5-nitro-1H-imidazole-1 ethanol), which method comprises 2-dimethyl- 5-nitro-imidazole is reacted with propylene oxide, and the reactant is suspended in an organic ester solvent at a temperature range of 0-5, and the formed butynidazole is separated from the mixture by a conventional method. The other butinidazole prepared by the method of the invention has high purity and high yield, and is a high-efficiency anti-amoeba and antigen biomedicine.

Description

technical field [0001] The present invention relates to a method for preparing another butinidazole (i.e. 2-dimethyl-5-nitro-1H-imidazole-1 ethanol, i.e. 1-(2-hydroxypropyl)-2-methyl-5-nitro -1H-imidazole) improved method. The albunidazole prepared by the method of the present invention has a structure as shown in general formula I; it is a high-efficiency anti-amoeba and antigen biomedicine. [0002] [0003] Formula I technical background [0004] In addition, butinidazole is a high-efficiency anti-amoeba and antigen biological drug, and its demand is growing rapidly. Therefore, it is necessary to develop a novel high-yield and low-cost method. [0005] The synthesis of other butinidazole was initially reported by Rhone-poulec S.A (referring to French patent 1427627 (on October 10, 1963) and French patent M3270 (on December 30, 1963)), they involved the 2- Methyl-5-nitro-imidazole (1 mol) was dissolved in a large amount of formic acid (85%) (7.88 parts). To the abo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D233/91
Inventor A·V·瑞缔T·M·索纳尔S·A·德施潘得
Owner UNICHEM LAB LTD
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