Sulfuric Acid → HCID 54211560, Verbindung

HRID 1532615

Reaktionsgleichung

Reaktionsgleichung von HRID 1532615
[CH3:1][C:2]([CH3:10])([CH3:9])[CH2:3][C@@H:4]([C:6]([OH:8])=[O:7])[NH2:5].S(=O)(=O)(O)O.[CH3:16][C:17](=[CH2:19])[CH3:18].[OH-].[Na+]>C(OCC)(=O)C.O1CCOCC1>[C:17]([O:7][C:6](=[O:8])[C@H:4]([CH2:3][C:2]([CH3:10])([CH3:9])[CH3:1])[NH2:5])([CH3:19])([CH3:18])[CH3:16]

Komponenten

7

Edukt 4

HCID 1118Sulfuric AcidHCID 8255IsobutyleneHCID 14798Sodium Hydroxide2×HCID 194032(2S)-2-Amino-4,4-dimethylpentanoic acid

Produkt 1

HCID 54211560HCID 54211560, VerbindungAusbeute 50,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8857Ethyl AcetateLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

To a pressure bottle were added 1.5 gm (10.3 mMol) 4-methyl-(L)-leucine, 25 mL dioxane, 1.5 mL concentrated sulfuric acid and 25 mL isobutylene. The pressure bottle was stoppered and the reactants were shaken together for 18 hours. The reaction mixture was then treated with 60 mL cold 1N sodium hydroxide and 100 mL ethyl acetate. To this mixture was added sufficient 1N sodium hydroxide until the pH of the mixture was 8.5. The layers were separated and the aqueous phase was extracted well with ethyl acetate. The combined ethyl acetate phases were dried over sodium sulfate and concentrated under reduced pressure to provide an oil which gradually crystallized to provide 1.05 gm (50.5%) of the title compound.

Aufarbeitung

  1. customThe layers were separated
  2. extractionthe aqueous phase was extracted well with ethyl acetate
  3. dry with materialThe combined ethyl acetate phases were dried over sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto provide an oil which
  6. customgradually crystallized

Quellen und Nachweise

ORD-Eintrag
ord-ef4a455f646e40f5a2c700c3821061fc
Quelldatensatz
uspto-grants-2001_03
Patentnummer
US06204260B1

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