Cesium carbonate → HCID 86681327, Verbindung

HRID 1778920Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1778920
[O:1]1[C:3]2([CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]2)[CH2:2]1.[CH3:10][C:11]1[NH:15][C:14]([C:16]#[N:17])=[CH:13][CH:12]=1.C([O-])([O-])=O.[Cs+].[Cs+]>CN(C)C=O.C(OCC)(=O)C>[OH:1][C:3]1([CH2:2][N:15]2[C:11]([CH3:10])=[CH:12][CH:13]=[C:14]2[C:16]#[N:17])[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1

Komponenten

6

Edukt 3

HCID 10796Cesium carbonateHCID 5706055-Methyl-1H-pyrrole-2-carbonitrileHCID 6429411-Oxaspiro(2.6)nonane

Produkt 1

HCID 86681327HCID 86681327, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

1-Oxaspiro[2,6]nonane (2.5 g), 5-methyl-1H-pyrrole-2-carbonitrile (2.1 g) and Cs2CO3 (6.45 g) in N,N-dimethylformamide (15 mL) was heated at 120° C. in a Biotage Initiator microwave reactor for 30 minutes. The reaction mixture was diluted with ethyl acetate, washed with water and concentrated. The residue was purified by reverse phase chromatography, and was eluted with 30%-70% acetonitrile in 0.1% TFA water solution to provide the title compound.

Aufarbeitung

  1. washwashed with water
  2. concentrationconcentrated
  3. customThe residue was purified by reverse phase chromatography
  4. washwas eluted with 30%-70% acetonitrile in 0.1% TFA water solution

Quellen und Nachweise

ORD-Eintrag
ord-c56891ea55ca4501999b575e23ef7b9a
Quelldatensatz
uspto-grants-2016_02
Patentnummer
US09266877B2

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