Sodium Hydroxide → 3,4-Dichloro-N'-hydroxybenzene-1-carboximidamide

HRID 1497027Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1497027
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[Cl:10])[C:5]#[N:6].Cl.[NH2:12][OH:13].[OH-].[Na+]>C(O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[Cl:10])/[C:5](=[N:12]/[OH:13])/[NH2:6]

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 810513,4-DichlorobenzonitrileHCID 443297Hydroxyamine hydrochloride

Produkt 1

HCID 112641853,4-Dichloro-N'-hydroxybenzene-1-carboximidamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of 3,4-dichlorobenzonitrile (2.00 g, 11.6 mmol), hydroxylamine hydrochloride (1.65 mL, 12.8 mmol) and sodium hydroxide (4.15 mL, 12.4 mmol) in ethanol (40 mL) was stirred at rt for 1 h. The reaction mixture was concentrated and refluxed in hexanes for 30 min and concentrated in vacuo. The product, intermediate 33A was used directly without purification. HPLC/MS (Method C) retention time=1.24 min [M+H]+204.9.

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated
  2. temperaturerefluxed in hexanes for 30 min
  3. concentrationconcentrated in vacuo
  4. customThe product, intermediate 33A was used directly without purification

Quellen und Nachweise

ORD-Eintrag
ord-f4a465105da645639c3b9a45d21426d2
Quelldatensatz
uspto-grants-2015_12
Patentnummer
US09199946B2

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