Cesium fluoride → HCID 22498336, Verbindung

HRID 984503Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 984503
[NH:1]1[CH2:13][CH2:12][CH2:11][CH:3]([C:4]([O:6][C:7]([CH3:10])([CH3:9])[CH3:8])=[O:5])[CH2:2]1.F[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[N+:21]([O-:23])=[O:22].[F-].[Cs+]>C1(C)C=CC=CC=1.C(OCC)(=O)C>[N+:21]([C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=1[N:1]1[CH2:13][CH2:12][CH2:11][CH:3]([C:4]([O:6][C:7]([CH3:9])([CH3:10])[CH3:8])=[O:5])[CH2:2]1)([O-:23])=[O:22]

Komponenten

6

Edukt 3

HCID 25953Cesium fluorideHCID 738951-Fluoro-2-nitrobenzeneHCID 42271713-Piperidinecarboxylic acid t-butyl ester HCl

Produkt 1

HCID 22498336HCID 22498336, VerbindungAusbeute 96,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1140TolueneLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a solution of Example 437C (10.4 g, 56.1 mmol) in toluene (112 mL) was added 2-fluoronitrobenzene (6.0 mL, 56 mmol) and CsF (852 mg, 5.6. mmol). The reaction mixture was stirred under reflux conditions for 18 h, and allowed to cool to ambient temperature. The mixture was diluted with ethyl acetate (100 mL), washed with 10% HCl (2×50 mL), followed by brine (3×100 mL), then dried (Na2SO4) and evaporated in vacuo to obtain the title compound (16.5 g, 94%). MS (ESI) m/e 307 (M+H)+.

Aufarbeitung

  1. washwashed with 10% HCl (2×50 mL)
  2. dry with materialdried (Na2SO4)
  3. customevaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-19767238f58047c89c8fdb090d7edeb8
Quelldatensatz
uspto-grants-2005_03
Patentnummer
US06867203B2

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