Water → HCID 57599641, Verbindung

HRID 1787541Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1787541
[OH:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[C:4]([N+:10]([O-:12])=[O:11])[C:3]=1[O:13][CH3:14].[CH3:15][O:16][CH2:17]Cl.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH3:14][O:13][C:3]1[C:4]([N+:10]([O-:12])=[O:11])=[C:5]([CH:8]=[CH:9][C:2]=1[O:1][CH2:15][O:16][CH3:17])[C:6]#[N:7]

Komponenten

6

Edukt 4

HCID 962WaterHCID 7864Chloromethyl Methyl EtherHCID 11430Potassium CarbonateHCID 70592654-hydroxy-3-methoxy-2-nitrobenzonitrile

Produkt 1

HCID 57599641HCID 57599641, VerbindungAusbeute 84 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

A mixture of 4-hydroxy-3-methoxy-2-nitrobenzonitrile 1.00 g, chloromethyl methyl ether 0.47 mL (6.18 mmol) and potassium carbonate 3.56 g (25.8 mmol) in N,N-dimethylformamide 10 mL was stirred at 50° C. for 2 hours. The reaction mixture was poured into water and extracted into diethyl ether. The organic layer was washed with brine, dried over MgSO4, filtrated and the solvent was evaporated. Silica gel chromatography (n-hexane/AcOEt=4/1) afforded the title compound 1.03 g as colorless solid. Yield 83.5%.

Aufarbeitung

  1. extractionextracted into diethyl ether
  2. washThe organic layer was washed with brine
  3. dry with materialdried over MgSO4
  4. filtrationfiltrated
  5. customthe solvent was evaporated

Quellen und Nachweise

ORD-Eintrag
ord-930fcbcc989644c685589bbc369dfca5
Quelldatensatz
uspto-grants-2009_03
Patentnummer
US07511041B2

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