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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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  • 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 in the reaction system, can react violently with alkali, decompose violently, produce a large amount of heat and thick smoke, even exploded
There are huge security problems in actual production

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
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Add 0.01mol 2-p-ethoxyanilino-4-nitrobenzoic acid and 0.02mol phosphorus oxychloride to a 100ml round bottom flask, reflux at 90°C for 1 hour, add N,N-dimethyl Dimethicone solvent washing, then suction filtration, and then washing with water and suction filtration to obtain 2-ethoxy-6-nitro-9-chloroacridine with a yield of 99%.

[0035] (2) Add 0.01mol 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 , 0.02 mol of ethylene glycol, 0.1 mol of ammonia gas was introduced at 0°C, reacted at 100°C for 2 hours, and filtered to obtain 2-ethoxy-6-nitro-9-aminoacridine with a yield of 92%.

Embodiment 2

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

Embodiment 3

[0039] In step (1), reflux reaction at 120° C. for 0.5 h, 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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