Water → 4-Chloro-2-[[(1-methylethylidene)amino]oxy]benzonitrile

HRID 1292522Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1292522
[CH3:1][C:2](=[N:4][OH:5])[CH3:3].[K].[Cl:7][C:8]1[CH:15]=[CH:14][C:11]([C:12]#[N:13])=[C:10]([N+]([O-])=O)[CH:9]=1.O>CN(C)C=O>[Cl:7][C:8]1[CH:15]=[CH:14][C:11]([C:12]#[N:13])=[C:10]([O:5][N:4]=[C:2]([CH3:3])[CH3:1])[CH:9]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 67180Acetone, oximeHCID 969244-Chloro-2-nitrobenzonitrileHCID 5462222Potassium

Produkt 1

HCID 187964524-Chloro-2-[[(1-methylethylidene)amino]oxy]benzonitrileAusbeute 65,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

In 75 ml of dry N,N-dimethylformamide was dissolved acetone oxime (1.21 g), followed by potassium tertiaryl butoxide (1.85 g) and stirred under nitrogen. After 30 minutes, 4-chloro-2-nitro-benzonitrile (2.00 g) was added. After an additional 30 minutes the reaction was poured into water (500 ml) and filtered. The solid was collected and dissolved in DCM (250 ml), dried (MgSO4), and concentrated in vacuo. The resulting solid was recrystallized from ethanol to yield 1.5 g of the product, m.p. 83°-84° C.

Aufarbeitung

  1. filtrationfiltered
  2. customThe solid was collected
  3. dissolutiondissolved in DCM (250 ml)
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. customThe resulting solid was recrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-82a6f70c71924a3db37502bafd87e359
Quelldatensatz
uspto-grants-1998_05
Patentnummer
US05756754

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