Hydrochloric Acid → Minocycline Hydrochloride Dihydrate

HRID 1590328

Reaktionsgleichung

Reaktionsgleichung von HRID 1590328
[CH3:1][N:2]([C:4]1[C:9]2[CH2:10][C@@H:11]3[C:21]([C:22](=[O:23])[C:8]=2[C:7]([OH:33])=[CH:6][CH:5]=1)=[C:20]([OH:24])[C@@:19]1([OH:25])[C@H:13]([C@H:14]([N:30]([CH3:32])[CH3:31])[C:15]([OH:29])=[C:16]([C:26]([NH2:28])=[O:27])[C:17]1=[O:18])[CH2:12]3)[CH3:3].[OH2:34].[ClH:35].C(N(CC(O)=O)CC(O)=O)CN(CC(O)=O)CC(O)=[O:41]>CO>[CH3:32][N:30]([C@@H:14]1[C:15](=[O:29])[C:16]([C:26]([NH2:28])=[O:27])=[C:17]([OH:18])[C@:19]2([OH:25])[C@H:13]1[CH2:12][C@H:11]1[C:21]([C:20]2=[O:24])=[C:22]([OH:23])[C:8]2[C:9](=[C:4]([N:2]([CH3:3])[CH3:1])[CH:5]=[CH:6][C:7]=2[OH:33])[CH2:10]1)[CH3:31].[OH2:41].[OH2:34].[ClH:35]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 6049Ethylenediaminetetraacetic AcidHCID 178482881HCID 178482881, Verbindung

Produkt 1

HCID 68858974Minocycline Hydrochloride DihydrateAusbeute 99,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

Ten grams of a crude minocycline [HPLC. purity, 94.8% (percentage area)] was suspended at 15° to 20° C. in a mixed solvent of 30 ml of water and 45 ml of methanol and dissolved at a pH of 0.8 to 1.0 by adding conc. hydrochloric acid with stirring. Subsequently, 1 g of activated carbon and 10 mg of EDTA.2Na were added, and after 30 minutes' stirring, the activated carbon was separated by filtration. To the filtrate was added dropwise a 5% aqueous sodium hydroxide solution to adjust the pH of the filtrate to 4.0, whereby minocycline precipitated in the form of a hydrochloride. This hydrochloride was separated by filtration and dried in vacuo to obtain 11.0 g of a purified minocycline hydrochloride dihydrate [HPLC. purity, 99.4% (area percentage)].

Aufarbeitung

  1. dissolutiondissolved at a pH of 0.8 to 1.0
  2. addition2Na were added
  3. stirringafter 30 minutes' stirring
  4. customthe activated carbon was separated by filtration
  5. additionTo the filtrate was added dropwise a 5% aqueous sodium hydroxide solution
  6. customprecipitated in the form of a hydrochloride
  7. customThis hydrochloride was separated by filtration
  8. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-ac9c35d74dc54f7cae45f6156a073abe
Quelldatensatz
uspto-grants-1993_04
Patentnummer
US05202449

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