Pyridine → Benzophenone oxime

HRID 273668

Reaktionsgleichung

Reaktionsgleichung von HRID 273668
[C:1]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[NH2:16][OH:17].N1C=CC=CC=1>C(O)C>[C:1](=[N:16][OH:17])([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 3102BenzophenoneHCID 443297Hydroxyamine hydrochloride

Produkt 1

HCID 11324Benzophenone oximeAusbeute 73 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of benzophenone (10.0 g), hydroxylamine hydrochloride (10.0 g), pyridine (50 ml), and absolute ethanol (50 ml) was pumped through the CMR (15 ml/min; 155°-60° C., 700 kPa). The effluent was cooled and the solvent removed by rotary evaporation, and the residue stirred with cold water (50 ml). The crued oxime was filtered off and recrystallised from ethanol to afford pure product (8.0 g; 73% yield), m.p. 140.5°-141° C., cf lit.5 for a batchwise preparation by microwave heating.

Aufarbeitung

  1. customwas pumped through the CMR (15 ml/min; 155°-60° C., 700 kPa)
  2. temperatureThe effluent was cooled
  3. customthe solvent removed by rotary evaporation
  4. filtrationThe crued oxime was filtered off
  5. customrecrystallised from ethanol
  6. customto afford pure product (8.0 g; 73% yield), m.p. 140.5°-141° C., cf lit.5
  7. customfor a batchwise preparation by microwave
  8. temperatureheating

Quellen und Nachweise

ORD-Eintrag
ord-ac558e05036749a489f53ea207276d67
Quelldatensatz
uspto-grants-1995_02
Patentnummer
US05387397

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