Hydrazine hydrate (1:1) → 2-Ethoxybenzhydrazide

HRID 1794582

Reaktionsgleichung

Reaktionsgleichung von HRID 1794582
[CH2:1]([O:3][C:4]1[CH:14]=[CH:13][CH:12]=[CH:11][C:5]=1[C:6](OCC)=[O:7])[CH3:2].O.[NH2:16][NH2:17]>C(O)C>[CH2:1]([O:3][C:4]1[CH:14]=[CH:13][CH:12]=[CH:11][C:5]=1[C:6]([NH:16][NH2:17])=[O:7])[CH3:2]

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)2×HCID 221644Benzoic acid, 2-ethoxy-, ethyl ester

Produkt 1

HCID 1407882-Ethoxybenzhydrazide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Ethyl 2-ethoxybenzoate (100 g, 128.7 mmol) and hydrazine hydrate (100%, 25 ml, 128.7 mmol) are dissolved in 200 ml of ethanol and heated under reflux for 5 hours. A further 12.5 ml (64.3 mmol) of hydrazine hydrate are added and the reaction mixture is heated under reflux for a further 7 hours. For working up, the reaction mixture is extensively concentrated and then stirred with 300 ml of cyclohexane at room temperature. After cooling to 0° C., the crystals are filtered off with suction, washed twice with 50 ml of cold cyclohexane each time and finally dried in a vacuum oven at 35° C. and 300 mbar overnight.

Aufarbeitung

  1. temperatureheated
  2. temperatureunder reflux for 5 hours
  3. temperaturethe reaction mixture is heated
  4. temperatureunder reflux for a further 7 hours
  5. concentrationthe reaction mixture is extensively concentrated
  6. temperatureAfter cooling to 0° C.
  7. filtrationthe crystals are filtered off with suction
  8. washwashed twice with 50 ml of cold cyclohexane each time
  9. customfinally dried in a vacuum oven at 35° C.
  10. custom300 mbar overnight

Quellen und Nachweise

ORD-Eintrag
ord-6c73366988844741950c23fb20734acd
Quelldatensatz
uspto-grants-2006_04
Patentnummer
US07022847B2

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