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Preparation method of phacolysin

A technology of facolin and diaminophenazine, applied in the field of medicine, can solve problems such as difficulties in industrialization

Inactive Publication Date: 2014-11-19
JIANGXI ZETONG PHARMA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The second step of synthesis is to add o-phenylenediamine to the product of the first step, 2,3-diaminophenazine, and reflux in benzyl alcohol solution to generate the intermediate 5,12-dihydro-5,7,12,14- Tetrazolium, the next step is to use chlorosulfonic acid for sulfonation, and at the same time, the product is finally purified by neutral alumina column chromatography to obtain falkolin, which brings difficulties to industrialization

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0021] Add 150 g of o-phenylenediamine to 7000 ml of water, and add 234 ml of concentrated hydrochloric acid dropwise under stirring to dissolve it. FeCl 3 ·6H 2 Dissolve 1120g of O in 2100ml of water, add this solution dropwise to the o-phenylenediamine hydrochloric acid solution at 20-30°C under stirring, and finish the addition in about 1 hour, then continue to stir for 2 hours and let it stand overnight, filter the next day, and filter the cake with 10-15 ℃ Wash with 1400ml of 0.3N hydrochloric acid for three times, drain, dissolve the filter cake in 4900-5600ml of boiling distilled water, adjust the pH to 7-8 with 50% KOH, filter, wash the filter cake with water for 3 times, and dry at 70-80℃ That is: 63.0g, yield: 86.4%.

[0022] In a 2000ml three-necked flask, add 180g of 2,3-diaminophenazine and 135g of o-phenylenediamine, add 1700ml of benzyl alcohol, stir and reflux for 2h under heating conditions, cool down to below 100°C, add 6.75g of concentrated sulfuric acid (...

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Abstract

The invention discloses a preparation method of phacolysin. In the synthetic process of phacolysin, 5,12-dihydro-5,7,12,14-azapentacene is sulphonated by using phosphorus pentoxide and a concentrated sulfuric acid, so that a high-concentration fuming sulphuric acid is prevented from being taken as a sulfonating agent; and in the refining and purifying process of phacolysin, a carboxylic weak acid type cation exchange resin is adopted for purifying products, so that high-purity phacolysin products are prepared.

Description

technical field [0001] The present invention belongs to the field of medicine, and relates to a method for synthesizing fakolin, specifically a method for preparing 5,12-dihydro-5,7,12,14-tetraazolene sulfonation and sulfonate sodium salt . Background technique [0002] Fakolin, chemical name: 5,12-dihydro-5,7,12,14-tetrazavalene-2,9-sodium disulfonate, used for primary senile cataract, traumatic cataract, Congenital cataract and secondary cataract also have a certain effect. The molecular formula of fakolin is: [0003] . [0004] The method used in Japanese Patent Laid-Open No. 49-109399 is: add 2,5-dimethoxy-1,4-benzoquinone and 1,2-sodium diaminobenzenesulfonate to the mixed solution of water and glacial acetic acid , stirred and reacted at 70°C for 1 hour, cooled at room temperature until crystals precipitated to form 5,12-dihydro-5,7,12,14-tetrazapentacene 2,9-sodium disulfonate, this synthetic method The characteristic of this method is that the route is short,...

Claims

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Application Information

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IPC IPC(8): C07D487/04
CPCC07D487/04
Inventor 钟劲松周国梁华峰
Owner JIANGXI ZETONG PHARMA CHEM