Preparation method of ethacridine lactate intermediate

A technology of ethacridine lactic acid and intermediates, which is applied in the field of preparation of ethacridine lactic acid intermediates, can solve problems such as explosion, and achieve the effects of increasing reaction yield, avoiding environmental pollution, and mild reaction conditions

Inactive Publication Date: 2012-11-21
BEIJING UNIV OF CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The problem that this method exists is that after the first step reaction finishes, need to adjust pH with lye, and because there is a large amount of phosphorus oxychloride residues i

Method used

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  • Preparation method of ethacridine lactate intermediate
  • Preparation method of ethacridine lactate intermediate
  • Preparation method of ethacridine lactate intermediate

Examples

Experimental program
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Example Embodiment

[0033] Example 1

[0034] (1) Add 0.01mol 2-p-ethoxyphenylamino-4-nitrobenzoic acid and 0.02mol phosphorus oxychloride into a 100ml round-bottom flask, and react at 90℃ under reflux for 1h. Add N,N-dimethyl After washing with methyl formamide solvent, then suction filtration, then washing with water and suction filtration, 2-ethoxy-6-nitro-9-chloroacridine was obtained with a yield of 99%.

[0035] (2) Add 0.01mol of 2-ethoxy-6-nitro-9-chloroacridine to a 100ml round bottom flask, add 40ml of N,N-dimethylformamide to dissolve, add 0.01mol of phosphorus oxychloride , 0.02mol of ethylene glycol, 0.1mol of ammonia gas at 0°C, reaction at 100°C for 2h, filtration to obtain 2-ethoxy-6-nitro-9-aminoacridine with a yield of 92%.

Example Embodiment

[0036] Example 2

[0037] In step (1), the reaction was refluxed at 70°C for 2 hours, and the other steps were the same as in Example 1, with a yield of 95%.

Example Embodiment

[0038] Example 3

[0039] In step (1), the reaction was refluxed at 120°C for 0.5 h, and the other steps were the same as in Example 1, and the yield was 94%.

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Abstract

The invention relates to a preparation method of an ethacridine lactate intermediate. The preparation method comprises the following steps that phosphorus oxychloride and 2-p-ethoxyphenylamino-4-nitrobenzoic acid are mixed according to a mole ratio of 2: 1; the mixture undergoes a reaction at a temperature of 70 to 120 DEG C for 0.5 to 2 hours; reaction products are cooled to a room temperature and are directly added with a polar aprotic solvent and a multi-fatty alcohol catalyst; the mixture is added with a nitrogen source at a low temperature of -10 to 20 DEG C; and the mixture with the nitrogen source is heated to a temperature of 80 to 180 DEG C and undergoes a reaction for 1 to 6 hours to produce 2-ethoxy-6-nitro-9-aminoacridine. The preparation method can be operated simply, is safe, realizes recovery and recycle of a reaction waste liquid thereby avoiding environmental pollution, reduces a raw material cost and improves a reaction yield.

Description

technical field [0001] The invention relates to a preparation method of a halogenated nitrogen-containing heterocyclic aromatic hydrocarbon, in particular to a preparation method of an ethacridine lactic acid intermediate. Background technique [0002] Ethacridine lactate is the lactate salt of ethacridine, 2-ethoxy-6,9-diaminoacridine. Ethacridine (EthacridineLactate) trade name is rivanol or rivonol, which is an acridine basic dye bactericidal antiseptic. It has a strong killing effect on Gram-positive bacteria and a small number of Gram-negative bacteria, and has a good antibacterial effect on cocci, especially streptococci. It is widely used in the treatment of various wounds and infectious skin diseases. In addition, ethacridine lactate has the effect of stimulating uterine muscles. Administration through the amniotic cavity and intrauterine cavity can cause decidual tissue necrosis in the uterus to produce endogenous prostaglandins, thereby causing uterine contraction...

Claims

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Application Information

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IPC IPC(8): C07D219/10
Inventor 乔仁忠张波王肇坤李淑梅王凤鸣王韧
Owner BEIJING UNIV OF CHEM TECH
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