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Hydrochloric Acid → Prostaglandin E2

HRID 1579716
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1579716
[OH:1]O.[CH3:3][CH2:4][CH2:5][CH2:6][CH2:7][C@H:8]([OH:26])/[CH:9]=[CH:10]/[C@@H:11]1[C@@H:16]([CH2:17]/[CH:18]=[CH:19]\[CH2:20][CH2:21][CH2:22][C:23]([OH:25])=[O:24])[C:14](=[O:15])[CH:13]=[CH:12]1.[OH-].[Na+].Cl>CO>[CH3:3][CH2:4][CH2:5][CH2:6][CH2:7][C@H:8]([OH:26])/[CH:9]=[CH:10]/[C@@H:11]1[C@@H:16]([CH2:17]/[CH:18]=[CH:19]\[CH2:20][CH2:21][CH2:22][C:23]([OH:25])=[O:24])[C:14](=[O:15])[CH2:13][C@H:12]1[OH:1].[CH3:3][CH2:4][CH2:5][CH2:6][CH2:7][C@H:8]([OH:26])/[CH:9]=[CH:10]/[C@@H:11]1[C@@H:16]([CH2:17]/[CH:18]=[CH:19]\[CH2:20][CH2:21][CH2:22][C:23]([OH:25])=[O:24])[C:14](=[O:15])[CH2:13][C@@H:12]1[OH:1]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 5280880Pga2

Produkt 2

HCID 5280360Prostaglandin E2HCID 528306111beta-PGE2

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887
Methanol
Lösungsmittel

Reaktionsbedingungen

Temperatur
-20 °C

Versuchsvorschrift

Hydrogen peroxide (0.35 ml.; 30% aqueous) is added to a solution of PGA2 (200 mg.) in 5 ml. of methanol. The mixture is cooled to -20°C., and 0.75 ml. of one N aqueous sodium hydroxide solution is slowly added with stirring. After one hour of stirring at -20°C., 1 ml. of one N hydrochloric acid is added, and the mixture is evaporated under reduced pressure. The residue is dissolved in ethyl acetate, and the resulting solution is washed successively with water and brine, dried with anhydrous sodium sulfate, and evaporated. The residue is treated with amalgamated aluminum as described in Example 8, using 2.5 ml. diethyl ether, 0.25 ml. methanol, and 0.03 ml. water, the amalgamated aluminum being added in 2 portions. When the reduction is complete, ethyl acetate and one N hydrochloric acid are added to the reaction mixture and the mixture is separated in a separatory funnel. The ethyl acetate layer is washed successively with one N hydrochloric acid, water, and brine, dried with anhydrous sodium sulfate, and evaporated. The residue is subjected to preparative thin layer chromatography to give PGE2 and 11β-PGE2 in the ratio 1:2.

Aufarbeitung

  1. stirringAfter one hour of stirring at -20°C.
  2. customthe mixture is evaporated under reduced pressure
  3. dissolutionThe residue is dissolved in ethyl acetate
  4. washthe resulting solution is washed successively with water and brine
  5. dry with materialdried with anhydrous sodium sulfate
  6. customevaporated
  7. additionThe residue is treated with amalgamated aluminum
  8. additionwater, the amalgamated aluminum being added in 2 portions
  9. additionethyl acetate and one N hydrochloric acid are added to the reaction mixture
  10. customthe mixture is separated in a separatory funnel
  11. washThe ethyl acetate layer is washed successively with one N hydrochloric acid, water, and brine
  12. dry with materialdried with anhydrous sodium sulfate
  13. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-71f47d80692747d580b7fe8110168660
Quelldatensatz
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US03931283

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