Acetic Acid → HCID 11276149, Verbindung

HRID 2240609Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2240609
C[O:2][C:3](=O)[CH2:4][CH2:5][C:6]1[C:7](=[O:15])[N:8]([CH2:12][CH:13]=[CH2:14])[CH2:9][CH2:10][CH:11]=1.[NH2:17][O:18][K].C(O)(=O)C>CO.C(OCC)(=O)C>[CH2:12]([N:8]1[CH2:9][CH2:10][CH:11]=[C:6]([CH2:5][CH2:4][C:3]([NH:17][OH:18])=[O:2])[C:7]1=[O:15])[CH:13]=[CH2:14]

Komponenten

6

Edukt 3

HCID 176Acetic AcidHCID 167205483-(1-Allyl-2-oxo-1,2,5,6-tetrahydro-pyridin-3-yl)-propionic acid methyl esterHCID 178514655HCID 178514655, Verbindung

Produkt 1

HCID 11276149HCID 11276149, VerbindungAusbeute 48 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

24 mg of 3-(1-allyl-2-oxo-1,2,5,6-tetrahydro-pyridin-3-yl)-propionic acid methyl ester (i1) prepared from the above Step 2 was dissolved in methanol solution (0.11 mM) and then 0.122 ml of 1.7M NH2OK suspension solution (0.207 mM) was added thereto at 0° c. and stirred for 3 hrs at room temperature. The resulting mixture was neutralized with 0.02 ml of acetic acid, diluted with 10 ml of ethyl acetate solution, filtered and concentrated in vacuo. The resulting compound was purified by column chromatography on Silica gel with methanol/chloroform (1:10) solvent mixture as an eluant to give 11 mg of the title compound (j1) (yield: 48%).

Aufarbeitung

  1. customat 0°
  2. filtrationfiltered
  3. concentrationconcentrated in vacuo
  4. customThe resulting compound was purified by column chromatography on Silica gel with methanol/chloroform (1:10) solvent mixture as an eluant

Quellen und Nachweise

ORD-Eintrag
ord-5cb32b194c12456da4e597e80b663639
Quelldatensatz
uspto-grants-2010_05
Patentnummer
US07723376B2

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