Methanol → HCID 13772856, Verbindung

HRID 344229Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 344229
[C:1]1([C@@H:7]([N:9]2[C:13](=[O:14])[CH2:12][C@H:11]([C:15]([OH:17])=[O:16])[CH2:10]2)[CH3:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.S(=O)(=O)(O)O.[CH3:23]O>>[C:1]1([C@@H:7]([N:9]2[C:13](=[O:14])[CH2:12][C@H:11]([C:15]([O:17][CH3:23])=[O:16])[CH2:10]2)[CH3:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Komponenten

4

Edukt 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 723630(3S)-5-oxo-1-[(1S)-1-phenylethyl]pyrrolidine-3-carboxylic acid

Produkt 1

HCID 13772856HCID 13772856, Verbindung

Versuchsvorschrift

(3S)-1-((S)-1-Phenylethyl)-5-oxo-3-pyrrolidinecarboxylic acid (666 g, optical purity not less than 99%) was dissolved in methanol (6 l), and conc. sulfuric acid (15 ml) was added at room temperature. The mixture was stirred at refluxing temperature for 7 hr. Methanol was evaporated, and the residue was extracted with ethyl acetate. The organic layer was washed with sodium hydrogencarbonate, dried over magnesium sulfate and concentrated under reduced pressure to give 738 g of methyl (3S)-1-((S)-1-phenylethyl)-5-oxo-3-pyrrolidine-carboxylate.

Aufarbeitung

  1. temperatureat refluxing temperature for 7 hr
  2. customMethanol was evaporated
  3. extractionthe residue was extracted with ethyl acetate
  4. washThe organic layer was washed with sodium hydrogencarbonate
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-737d2879531445e9bf38f47de4c0651f
Quelldatensatz
uspto-grants-1999_01
Patentnummer
US05864039

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