Water → HCID 18796452, Verbindung

HRID 582870

Reaktionsgleichung

Reaktionsgleichung von HRID 582870
[CH3:1][C:2](=[N:4][OH:5])[CH3:3].CC(C)([O-])C.[K+].[Cl:12][C:13]1[CH:20]=[CH:19][C:16]([C:17]#[N:18])=[C:15]([N+]([O-])=O)[CH:14]=1.O>CN(C)C=O>[Cl:12][C:13]1[CH:20]=[CH:19][C:16]([C:17]#[N:18])=[C:15]([O:5][N:4]=[C:2]([CH3:3])[CH3:1])[CH:14]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 67180Acetone, oximeHCID 969244-Chloro-2-nitrobenzonitrileHCID 23665647Potassium tert-butoxide

Produkt 1

HCID 18796452HCID 18796452, VerbindungAusbeute 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 tertiary 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-b0496799b6cd46ba84d9201c0b9b6e22
Quelldatensatz
uspto-grants-1999_07
Patentnummer
US05925766

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