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Process for preparing hexahydro pyridazine tricarboxylate

A technology of pyridazine tricarboxylate and sodium hydride, applied in directions such as organic chemistry, can solve problems such as expensive reagents and low product yield, and achieve the effects of improving reaction yield and product purity

Inactive Publication Date: 2005-08-17
LYNCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most of the existing methods require multiple steps, the reagents used are expensive, and the product yields are relatively low

Method used

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  • Process for preparing hexahydro pyridazine tricarboxylate
  • Process for preparing hexahydro pyridazine tricarboxylate

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Embodiment Construction

[0025] The present invention will be described in more detail below in conjunction with examples.

[0026] Raw material example

[0027] Preparation of ethyl 2,5-dibromopentanoate

[0028] Bromine (64.57 g, 99% purity, 0.40 mol) was added to delta-valerolactone (41.72 g, 96% purity, 0.40 mol) and PBr at a temperature of 110-115°C over 2 hours. 3 (2.20g, 0.008mol) below the liquid level of the mixed solution, wherein the second half needs to be added more slowly. After 60 minutes, the solution was cooled to 0-5°C and cold ethanol containing 3.65 g (0.10 mol) of dry HCl gas was added. After stirring at room temperature for 22 hours, ethanol and water were removed by distillation under reduced pressure (toluene or other suitable solvents can also be used to remove the water-ethanol azeotrope). The crude product was extracted with ether (200ml) and washed with saturated aqueous sodium bicarbonate (total 98ml, 0.124mol) to remove any unreacted acid. After removing the solvent b...

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PUM

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Abstract

The preparation process of hexahydro pyridazinyl tricarboxylate as shown in general expression I includes the reaction between 2, 5-bihalogeno valerate as shown in general expression II and hydrazine derivative as shown in general expression III in the presence of magnesium alcoholate. The hexahydro pyridazinyl tricarboxylat compound is one important medicine intermediate.

Description

technical field [0001] The invention relates to a preparation method of hexahydropyridazine tricarboxylate, in particular to a method for preparing hexahydropyridazine tricarboxylate in the presence of magnesium alkoxide and sodium hydride. Background technique [0002] Hexahydropyridazinetricarboxylic acid and its derivatives are extremely important intermediates for the synthesis of unnatural amino acids and peptidomimetics. Various methods for synthesizing hexahydropyridazinetricarboxylic acid and its derivatives have been disclosed in the prior art. However, most of the existing methods require multiple steps, the reagents used are expensive, and the product yields are relatively low. Contents of the invention [0003] The object of this invention is to provide a kind of method for preparing hexahydropyridazine tricarboxylate shown in following general formula (I): [0004] [0005] The method comprises the step of reacting 2,5-dihalogenated valerates represented ...

Claims

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Application Information

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IPC IPC(8): C07D237/04
Inventor 陈荣业李成斌
Owner LYNCHEM
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