Ammonium Hydroxide → 4-Chloro-3-hydroxybenzamide

HRID 2236521Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2236521
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](Cl)=[O:7])=[CH:4][C:3]=1[OH:11].[OH-].[NH4+:13]>O>[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH2:13])=[O:7])=[CH:4][C:3]=1[OH:11]

Komponenten

4

Edukt 2

HCID 14923Ammonium HydroxideHCID 754648184-Chloro-3-hydroxybenzoyl chloride

Produkt 1

HCID 451201374-Chloro-3-hydroxybenzamideAusbeute 86 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

4-Chloro-3-hydroxy-benzoyl chloride is cooled to 0° C. and 20 ml of ammonium hydroxide were added within 5 minutes. The mixture is allowed to stir at 0° C. for 30 minutes, then at room temperature for additional 30 minutes. 30 ml of water is added to the mixture and the white precipitate is filtered, the pH of the water layer is adjusted to 3, followed by extraction with ethyl acetate, dried over MgSO4 to give 4-chloro-3-hydroxy-benzamide as a white solid 850 mg (86% yield).

Aufarbeitung

  1. waitat room temperature for additional 30 minutes
  2. filtrationthe white precipitate is filtered
  3. extractionfollowed by extraction with ethyl acetate
  4. dry with materialdried over MgSO4

Quellen und Nachweise

ORD-Eintrag
ord-648c1bf9d84b402cbd7b32f4c8adb7a6
Quelldatensatz
uspto-grants-2010_05
Patentnummer
US07713994B2

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