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Acetonitrile → HCID 131730036, Verbindung

HRID 2067716
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2067716
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KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 5

HCID 6342Acetonitrile2×HCID 8857Ethyl AcetateHCID 81531DiisopropylethylamineHCID 15200286HCID 15200286, VerbindungHCID 594363011-(1,1-Dimethylethyl) (2S,4S)-4-(acetylthio)-1,2-pyrrolidinedicarboxylate

Produkt 1

HCID 131730036
HCID 131730036, Verbindung
Ausbeute 73,1 %

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A solution of 17.9 g (30 mmol) of p-nitrobenzyl(4R,5S,6S)-3-(diphenoxy-phosphoryloxy)-6-[(1R)-1-hydroxyethyl]-4-methyl-7-oxo-1-aza-bicyclo[3.2.0]hept-2-ene-2-carboxylate in 150 ml of acetonitrile was added into a flask and the reaction mixture was cooled below −10° C. Then diisopropylethylamine (8 mL) and a solution of the intermediate (I-1) prepared by Intermediate Example 1 (10.1 g, 31 mmol) in 100 mL of acetonitrile were added and the reaction mixture was stirred at 0° C. for 15 hours. After the completion of the reaction, ethyl acetate (400 mL) was added to the reaction mixture for dilution and the mixture was washed successively with water and saturated brine. The organic layer was dried and concentrated to give 14.7 g (yield: 73.1%) of p-nitrobenzyl (4R,5S,6S)-3-[(2S,4S)-2-formyl[[furan-2-ylmethyl]amino]-1-(tert-butoxycarbonyl)pyrrolidine-4-yl]thio-6-[(1R)-1-hydroxyethyl]-4-methyl-7-oxo-1-aza-bicyclo[3.2.0]hept-2-ene-2-carboxylate, which is the intermediate II-1.

Aufarbeitung

  1. temperaturethe reaction mixture was cooled below −10° C
  2. additionwere added
  3. additionwas added to the reaction mixture for dilution
  4. washthe mixture was washed successively with water and saturated brine
  5. customThe organic layer was dried
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-8e7a9f9c712f491ab400bbc044f953b8
Quelldatensatz
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08293895B2

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