Hydrochloric Acid → HCID 136271466, Verbindung

HRID 1391329Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1391329
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=O)[C:9]2[CH:14]=[C:13]([CH2:15][CH3:16])[CH:12]=[CH:11][C:10]=2[OH:17])=[CH:4][CH:3]=1.[OH-:19].[K+].Cl.[NH2:22]O.Cl>O.C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[N:22][OH:19])[C:9]2[CH:14]=[C:13]([CH2:15][CH3:16])[CH:12]=[CH:11][C:10]=2[OH:17])=[CH:4][CH:3]=1

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 12562655(4-Chlorophenyl)(5-ethyl-2-hydroxyphenyl)methanone

Produkt 1

HCID 136271466HCID 136271466, VerbindungAusbeute 43,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

4'-Chloro-5-ethyl-2-hydroxybenzophenone (65.2 g) and potassium hydroxide (170 g) in water (700 ml) and ethanol (150 ml.) were treated with hydroxylamine hydrochloride (70.0 g), with cooling, and the resulting mixture was stirred for 18 hours at ambient temperature. Dissolution occurred during this time. The solution was acidified with 5N-hydrochloric acid and then extracted with ether (3 × 200 ml.). The combined ether solutions were washed with 10% aqueous sodium carbonate solution (2 × 200 ml.) and evaporated to dryness to give an off-white solid. This solid was recrystallised from 40% benzene/60°-80° C. petrol ether to give a white crystalline solid (29.9 g), second crop (14.5 g) m.p. 117° C.

Aufarbeitung

  1. temperaturewith cooling
  2. dissolutionDissolution
  3. extractionextracted with ether (3 × 200 ml.)
  4. washThe combined ether solutions were washed with 10% aqueous sodium carbonate solution (2 × 200 ml.)
  5. customevaporated to dryness
  6. customto give an off-white solid
  7. customThis solid was recrystallised from 40% benzene/60°-80° C. petrol ether

Quellen und Nachweise

ORD-Eintrag
ord-3ff28f8471b640ddb9c24c8148987b36
Quelldatensatz
uspto-grants-1979_02
Patentnummer
US04141995

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