Hydrochloric Acid → 3,5-dichloro-2-amino-N-(2-hydroxyethoxy)benzamide

HRID 558067Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 558067
[Cl:1][C:2]1[C:3]([NH2:13])=[C:4]([CH:9]=[C:10]([Cl:12])[CH:11]=1)[C:5]([O:7]C)=O.[NH2:14][O:15][CH2:16][CH2:17][OH:18].C[O-].[Na+].Cl>CO.O>[Cl:1][C:2]1[C:3]([NH2:13])=[C:4]([CH:9]=[C:10]([Cl:12])[CH:11]=1)[C:5]([NH:14][O:15][CH2:16][CH2:17][OH:18])=[O:7]

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 613050Methyl 2-amino-3,5-dichlorobenzoateHCID 3014186Ethanol, 2-(aminooxy)-HCID 10942334Sodium Methoxide

Produkt 1

HCID 866307723,5-dichloro-2-amino-N-(2-hydroxyethoxy)benzamide

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittel2×HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

9 g (40.9 mmol) of methyl 3,5-dichloro-2-aminobenzoate and 6.3 g (81.8 mmol) of 2-(aminooxy)ethanol are initially charged in 90 ml of methanol, and 22.1 g (122.7 mmol) of sodium methoxide as a 30% strength solution in methanol are added dropwise at 20° C. The mixture is stirred at 50° C. overnight. The mixture is cooled and poured onto 400 ml of water, and the pH is adjusted to 3 using 1 N hydrochloric acid. The mixture is extracted 3 times with in each case 150 ml of ethyl acetate and the extracts are dried with sodium sulphate and concentrated using a rotary evaporator.

Aufarbeitung

  1. temperatureThe mixture is cooled
  2. extractionThe mixture is extracted 3 times with in each case 150 ml of ethyl acetate
  3. dry with materialthe extracts are dried with sodium sulphate
  4. concentrationconcentrated
  5. customa rotary evaporator

Quellen und Nachweise

ORD-Eintrag
ord-f392fc23c3624e0bbbb713a5ea5747e4
Quelldatensatz
uspto-grants-2011_11
Patentnummer
US08062995B2

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