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Phosphate → (1R,5S,6S)-2-[(4R)-pyrrolidine-2-thion-4-ylthio]-6-[(1R)-1-hydroxyethyl]-1-methylcarbapen-2-em-3-carboxylic acid isobutyryloxymethyl ester

HRID 257288
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 257288
[C:1]([O:6][CH2:7][O:8][C:9]([C:11]1[N:15]2[C:16](=[O:28])[C@H:17]([C@H:18]([O:20][Si](C(C)(C)C)(C)C)[CH3:19])[C@H:14]2[C@@H:13]([CH3:29])[C:12]=1[S:30][C@H:31]1[CH2:35][NH:34][C:33](=[S:36])[CH2:32]1)=[O:10])(=[O:5])[CH:2]([CH3:4])[CH3:3].CN(C)C=O.F.[NH4+].P([O-])([O-])([O-])=O>CN1CCCC1=O>[C:1]([O:6][CH2:7][O:8][C:9]([C:11]1[N:15]2[C:16](=[O:28])[C@H:17]([C@H:18]([OH:20])[CH3:19])[C@H:14]2[C@@H:13]([CH3:29])[C:12]=1[S:30][C@H:31]1[CH2:35][NH:34][C:33](=[S:36])[CH2:32]1)=[O:10])(=[O:5])[CH:2]([CH3:3])[CH3:4]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 1061PhosphateHCID 6228DimethylformamideHCID 11103665(1R,5S,6S)-2-[(4R)-pyrrolidine-2-thion-4-ylthio]-6-[(1R)-1-t-butyldimethylsilyloxyethyl]-1-methylcarbapen-2-em-3-carboxylic acid isobutyryloxymethyl esterHCID 13685747Ammonium hydrogenfluoride

Produkt 1

HCID 9955020
(1R,5S,6S)-2-[(4R)-pyrrolidine-2-thion-4-ylthio]-6-[(1R)-1-hydroxyethyl]-1-methylcarbapen-2-em-3-carboxylic acid isobutyryloxymethyl ester
Ausbeute 91 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 13387N-methyl-2-pyrrolidoneLösungsmittel

Reaktionsbedingungen

Temperatur
20 °C

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 isobutyryloxymethyl ester (3 g), dimethylformamide (20 ml), N-methylpyrrolidone (7 ml) and ammonium hydrogenfluoride (1.21 g) is stirred at 20° C. for three days. The reaction mixture is poured into a phosphate buffer (pH 7.0), and the mixture is extracted with ethyl acetate. The aqueous layer is extracted with ethyl acetate, and the organic layers are combined, washed with water, dried, and concentrated under reduced pressure. The resulting residue is crystallized from a mixture of ethyl acetate and diisopropyl ether. To the resultant is added diisopropyl ether, and the precipitate is collected by filtration, and washed to give (1R,5S,6S)-2-[(4R)-pyrrolidine-2-thion-4-ylthio]-6-[(1R)-1-hydroxyethyl]-1-methylcarbapen-2-em-3-carboxylic acid isobutyryloxymethyl ester (2.17 g) as crystals.

Aufarbeitung

  1. extractionthe mixture is extracted with ethyl acetate
  2. extractionThe aqueous layer is extracted with ethyl acetate
  3. washwashed with water
  4. customdried
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting residue is crystallized from a mixture of ethyl acetate and diisopropyl ether
  7. additionTo the resultant is added diisopropyl ether
  8. filtrationthe precipitate is collected by filtration
  9. washwashed

Quellen und Nachweise

ORD-Eintrag
ord-d15255eae5ed479dbac0768ff8dfab88
Quelldatensatz
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05260438

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