Hydrazine hydrate (1:1) → 2-(2-Chlorophenoxy)Ethylamine

HRID 1760925Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1760925
[Cl:1][C:2]1[CH:21]=[CH:20][CH:19]=[CH:18][C:3]=1[O:4][CH2:5][CH2:6][N:7]1C(=O)C2=CC=CC=C2C1=O.O.NN>Cl>[Cl:1][C:2]1[CH:21]=[CH:20][CH:19]=[CH:18][C:3]=1[O:4][CH2:5][CH2:6][NH2:7]

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 27091102-[2-(2-chlorophenoxy)ethyl]-2,3-dihydro-1H-isoindole-1,3-dione

Produkt 1

HCID 27357882-(2-Chlorophenoxy)Ethylamine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Versuchsvorschrift

21.0 grams (0.071 ml) of N-[2-(2-chlorophenoxy)ethyl]phthalimide and 3.55 grams (0.071 mol) of hydrazine hydrate are dissolved in 70 ml of moisture-free alcohol for heating and diffusing over 45 minutes. And stirred with 20 ml 18% HCl heat for diffusing over 1.0 hour. Upon cooling, after filtrating the extracted solids, 20% NaOH is added to alkalize. The mixed solution's organic layer is extracted with chloroform and filtrating the extracted solids with potassium carbonate solution. The generated product is filled into silica gel columns utilizing the ratio of ethyl acetate as the diluent; upon purification, 2-(2-chlorophenoxy) ethylamine is obtained.

Aufarbeitung

  1. temperaturefor heating
  2. temperatureheat
  3. waitfor diffusing over 1.0 hour
  4. temperatureUpon cooling
  5. filtrationafter filtrating the extracted solids, 20% NaOH
  6. additionis added
  7. extractionThe mixed solution's organic layer is extracted with chloroform
  8. filtrationfiltrating the extracted solids with potassium carbonate solution
  9. additionThe generated product is filled into silica gel columns
  10. customupon purification

Quellen und Nachweise

ORD-Eintrag
ord-e46dac1163774738b5e3b287f5c278be
Quelldatensatz
uspto-grants-2005_01
Patentnummer
US06846826B2

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