Chlorotrimethylsilane → 4-(4-Trimethylsilyloxy-piperidin-1-yl)-3-fluoronitrobenzene

HRID 750905Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 750905
[O:1]=[C:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][C:9]=2[F:17])[CH2:4][CH2:3]1.C(N(CC)CC)C.[CH3:25][Si:26](Cl)([CH3:28])[CH3:27]>CN(C)C=O>[CH3:25][Si:26]([CH3:28])([CH3:27])[O:1][CH:2]1[CH2:3][CH2:4][N:5]([C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][C:9]=2[F:17])[CH2:6][CH2:7]1

Komponenten

5

Edukt 3

HCID 6397ChlorotrimethylsilaneHCID 8471TriethylamineHCID 37637811-(2-Fluoro-4-nitrophenyl)piperidin-4-one

Produkt 1

HCID 693102754-(4-Trimethylsilyloxy-piperidin-1-yl)-3-fluoronitrobenzeneAusbeute 86 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

The mixture of 4-(4-oxo-piperidin-1-yl)-3-fluoronitrobenzene (0.250 mol), triethylamine (1.250 mol), trimethylsilylchloride (0.750 mol) in dimethylformamide was heated at 70° C. for 24 h. The solvent was removed under vacuum and to the residual mass was extracted with the ethyl acetate water mixture. The combined organic layer was dried and after removal of the solvent afforded title compound as a solid in 86% yield.

Aufarbeitung

  1. customThe solvent was removed under vacuum and to the residual mass
  2. extractionwas extracted with the ethyl acetate water mixture
  3. customThe combined organic layer was dried
  4. customafter removal of the solvent

Quellen und Nachweise

ORD-Eintrag
ord-1257c62a67044f35b69da57fd762b085
Quelldatensatz
uspto-grants-2008_07
Patentnummer
US07405228B2

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