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Phosphate → HCID 10571982, Verbindung

HRID 257287
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 257287
[CH2:1]([O:4][C:5]([C:7]1[N:11]2[C:12](=[O:24])[C@H:13]([C@H:14]([O:16][Si](C(C)(C)C)(C)C)[CH3:15])[C@H:10]2[C@@H:9]([CH3:25])[C:8]=1[S:26][C@H:27]1[CH2:31][NH:30][C:29](=[S:32])[CH2:28]1)=[O:6])[CH:2]=[CH2:3].F.[NH4+].P([O-])([O-])([O-])=O>CN(C)C=O>[CH2:1]([O:4][C:5]([C:7]1[N:11]2[C:12](=[O:24])[C@H:13]([C@H:14]([OH:16])[CH3:15])[C@H:10]2[C@@H:9]([CH3:25])[C:8]=1[S:26][C@H:27]1[CH2:31][NH:30][C:29](=[S:32])[CH2:28]1)=[O:6])[CH:2]=[CH2:3]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 1061PhosphateHCID 10720094HCID 10720094, VerbindungHCID 13685747Ammonium hydrogenfluoride

Produkt 1

HCID 10571982HCID 10571982, VerbindungAusbeute 85,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A mixture of (1R,5S,6S)-2-[(4R)-pyrrolidine-2-thion-4-ylthio]-6-[(1R)-1-t-butyldimethylsilyloxyethyl]-1-methylcarbapen-2-em-3-carboxylic acid allyl ester (1.00 g), dimethylformamide (10 ml) and ammonium hydrogenfluoride (459 mg) is stirred at room temperature for three days. To the reaction solution is added a phosphate buffer (pH 7.0), and the mixture is extracted with ethyl acetate. The organic layer is washed with a phosphate buffer, and the washing and the phosphate buffer layer are combined, and extracted with ethyl acetate. The organic layers are combined, washed, dried and concentrated under reduced pressure. The resulting residue is crystallized from a mixture of ethyl acetate and n-hexane (2:1) to give (1R,5S,6S)-2-[(4R)-pyrrolidine-2-thion-4-ylthio]-6-[(1R)-1-hydroxyethyl]-1-methylcarbapen-2-em-3-carboxylic acid allyl ester (657 mg). The filtrate of the above crystallization is concentrated under reduced pressure, and the residue is purified by silica gel flash column chromatography (solvent; chloroform:ethanol= 30:1), and further crystallized from a mixture of ethyl acetate and n-hexane (2:1) to give (1R,5S,6S)-2-[(4R)-pyrrolidine-2-thion-4-ylthio]-6-[(1R)-1-hydroxyethyl]-1-methylcarbapen-2-em-3-carboxylic acid ally ester (24 mg).

Aufarbeitung

  1. extractionthe mixture is extracted with ethyl acetate
  2. washThe organic layer is washed with a phosphate buffer
  3. extractionextracted with ethyl acetate
  4. washwashed
  5. customdried
  6. concentrationconcentrated under reduced pressure
  7. customThe resulting residue is crystallized from a mixture of ethyl acetate and n-hexane (2:1)

Quellen und Nachweise

ORD-Eintrag
ord-73c691d501bb44519804e4cc65999fe5
Quelldatensatz
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05260438

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