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Refining of demethylchlortetracycline

阅读:436发布:2022-08-14

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1. THE PROCESS OF EXTRACTING DEMETHYLCHLORTETRACYCLINE FROM A FERMENTATION MASH CONTAINING THE SAMED WHICH COMPRISES ACIDIFYING THE MASH TO A PH OF BETWEEN ABOUT 0.5-2.5 WITH A MINERAL ACID SO AS TO SOLUBILIXE THE DEMETHYLCHLORTETRACYCLINE CONTAINED THEREIN, FILTERING THE MASH, CONTACTING THE ACID FILTRATE WITH FROM 0.5 TO 3% BY VOLUME OF A COMPOUND OF THE GROUP CONSISTING OF OXALIC ACID AND AMMONIUM OXALATE SO AS TO PRECIPITATE EXCESS CALCIUM IONS, ADDING TO THE DECALCIFIED ACID FILTRATE FROM ABOUT 0.5 MOLE TO ABOUT 3 MOLES PER MOLE OF DEMETHYLCHLORTETRACYCLINE OF A QUATERNARY AMMONIUM COMPOUND SELECTED FROM THE GROUP CONSISTING OF LONG CHAIN ALKYL TRIMETHYLAMMONIUM CHLORIDES AND AND DIALKYLDIMETHYLAMMONIUM CHLORIDES AS TO FORM AS DEMETHYLCHLORTETRACYCLINE-QUATERNARY AMMONIUM COMPLEX, RAISING THE PH OF THE ACID FILTRATE TO BETWEEN ABOUT 8 AND 12 WITH AN ALKALIM CONTACTING THE ACID FILTRATE WITH A METHYL ALKYL KETONE SOLVENT SO AS TO EXTRACT HE DEMETHYLCHLORTETRACYCLINE THEREFROM, SEPARATING THE SOLVENT EXTRACT, AND THEREAFTER ISOLATING THE DEMETHYLCHLORTETRACYCLINE FROM THE SOLVENT EXTRACT.
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