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Sodium Iodide → 4-[5-(4-cyano-3-fluoro-phenoxy)pentyloxy]-N,N-bis(1-methylethyl)benzamide

HRID 2209742
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2209742
[OH:1][C:2]1[CH:16]=[CH:15][C:5]([C:6]([N:8]([CH:12]([CH3:14])[CH3:13])[CH:9]([CH3:11])[CH3:10])=[O:7])=[CH:4][CH:3]=1.Br[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22]Cl.C(=O)([O-])[O-].[Cs+].[Cs+].[F:30][C:31]1[CH:38]=[C:37]([OH:39])[CH:36]=[CH:35][C:32]=1[C:33]#[N:34].[H-].[Na+].[I-].[Na+]>CN(C)C=O>[C:33]([C:32]1[CH:35]=[CH:36][C:37]([O:39][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][O:1][C:2]2[CH:16]=[CH:15][C:5]([C:6]([N:8]([CH:12]([CH3:14])[CH3:13])[CH:9]([CH3:10])[CH3:11])=[O:7])=[CH:4][CH:3]=2)=[CH:38][C:31]=1[F:30])#[N:34]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 6

HCID 5238Sodium IodideHCID 10796Cesium carbonateHCID 24758Sodium hydrideHCID 960701-Bromo-5-chloropentaneHCID 27346752-Fluoro-4-hydroxybenzonitrileHCID 218414724-hydroxy-N,N-bis(propan-2-yl)benzamide

Produkt 1

HCID 19381499
4-[5-(4-cyano-3-fluoro-phenoxy)pentyloxy]-N,N-bis(1-methylethyl)benzamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

A stirred solution of 4-hydroxy-N,N-bis(1-methylethyl)benzamide (500 mg, 2.3 mmol) in 5 mL of N,N-dimethylformamide is treated with 1-bromo-5-chloropentane (300 μL, 2.3 mmol) and cesium carbonate (750 mg, 2.3 mmol) and heated for 2 hours. This is treated with a mixture of 2-fluoro-4-hydroxy-benzonitrile, and 60% sodium hydride (92 mg, 2.3 mmol) in 2 mL of N,N-dimethylformaide followed by sodium iodide (1.04 g, 6.9 mmol). The reaction is heated to 70° C. for 6 hours and partitioned between ethyl acetate and water. The organic phase is washed with brine, dried over sodium sulfate, and concentrated in vacuo. The resulting material is purified by chromatography on silica gel (20 g) with 70% ethyl acetate/hexane as the eluent to afford 4-[5-(4-cyano-3-fluoro-phenoxy)pentyloxy]-N,N -bis(1-methylethyl)benzamide.

Aufarbeitung

  1. temperatureheated for 2 hours
  2. custompartitioned between ethyl acetate and water
  3. washThe organic phase is washed with brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe resulting material is purified by chromatography on silica gel (20 g) with 70% ethyl acetate/hexane as the eluent

Quellen und Nachweise

ORD-Eintrag
ord-8966da142b98419c8f0b4b9ef2ab6e85
Quelldatensatz
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05455274

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