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Method for preparing 1,3-bicyclo hexyl barbituric acid

A technology of cyclohexylbarbituric acid and dicyclohexylurea is applied in the field of preparation of organic chemicals, can solve problems such as reversible loss of female fertility, and achieve the effects of easy operation, reduced production cost and high product yield

Inactive Publication Date: 2014-11-19
NANTONG HUAFENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The only clear adverse side effect currently identified for anti-angiogenic strategies is the reversible loss of female fertility

Method used

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  • Method for preparing 1,3-bicyclo hexyl barbituric acid
  • Method for preparing 1,3-bicyclo hexyl barbituric acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0016] Take a dry and clean 1L three-necked flask, add 150ml of glacial acetic acid into it, weigh 65.0g of N,N'-dicyclohexylurea (DCU) and add it directly into the three-necked flask, then weigh 33.0g of malonic acid and add In the three-necked flask, stir after adding, it becomes white and turbid, and the temperature rises to 70°C; measure 120ml of acetic anhydride, drop it into the three-necked flask with a dropping funnel, drop it within 1 hour, and keep warm at 35°C; the mixture is clearly solid-liquid, solid Clearly suspended in the clear liquid, after the dropwise addition, raise the temperature to 90°C, keep it warm for 5 hours, the color gradually deepens, from colorless to orange, and the reaction system changes from granular solid to flocculent turbidity; At about 30-40°C, a large amount of solids precipitated, and began to distill under reduced pressure in a water bath, and the vacuum degree was controlled at -0.08MPa; after evaporating to dryness, a brownish-yellow...

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Abstract

The invention discloses a method for preparing 1,3-bicyclo hexyl barbituric acid. The method comprises the following steps: reacting N,N'-dicyclohexyl urea and malonic acid in the presence of glacial acetic acid and acetic anhydride to generate 1,3-bicyclo hexyl barbituric acid, and further crystallizing, filtering, and drying, thereby obtaining refined 1,3-bicyclo hexyl barbituric acid. The method is reasonable in process structure, easy to operate and high in product yield, the purity of a product is high, the production cost is lowered, and the production benefits are increased.

Description

technical field [0001] The invention relates to a method for preparing organic chemicals, in particular to a method for preparing 1,3-bicyclohexylbarbituric acid. Background technique [0002] 1,3-Dicyclohexylbarbituric acid is the key intermediate of barbituric acid, which is mainly used in organic chemistry and medical fields. Barbituric acid can inhibit angiogenesis, tumorigenesis and proliferative diseases, and can also Used as a polymerization catalyst and a raw material for the preparation of dyes. [0003] Recent studies on angiogenesis inhibition have clearly demonstrated that effective inhibition of this process can block tumor growth in animal models. Perhaps the most striking example of the induction of tumor regression under experimental conditions using an anti-angiogenic strategy has recently been provided by studies using the natural polypeptides - angiostatin and endostatin. In addition to being clearly effective in these studies, there has been no toxicity...

Claims

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Application Information

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IPC IPC(8): C07D239/62
CPCC07D239/62
Inventor 王德峰张燕程张耀兵石飞
Owner NANTONG HUAFENG CHEM
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