Hydroxyamine hydrochloride → HCID 86733115, Verbindung

HRID 267550

Reaktionsgleichung

Reaktionsgleichung von HRID 267550
[N:1]([C:4]1[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][C:5]=1[C:6]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)=O)=[N+:2]=[N-:3].Cl.[NH2:20][OH:21]>N1C=CC=CC=1.C(O)C>[N:1]([C:4]1[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][C:5]=1[C:6](=[N:20][OH:21])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)=[N+:2]=[N-:3]

Komponenten

4

Edukt 2

HCID 443297Hydroxyamine hydrochlorideHCID 42128022-Azido-5-chlorobenzophenone

Produkt 1

HCID 86733115HCID 86733115, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21975839Pyridine ethanolLösungsmittel

Versuchsvorschrift

25.8 G (0.100 mol) of 2-azido-5-chlorobenzophenone [compare Example 1a] are dissolved in 500 ml of pyridine/ethanol (1:1). 14.0 G (0.200 mol) of hydroxylamine hydrochloride are added to the solution and the mixture is boiled for 5 hours under reflux and evaporated in vacuo at 60°C. The residue is taken up in 250 ml of methanol and the solution is poured into 250 ml of 2 N hydrochloric acid. The crude product which precipitates is filtered off, suspended in 250 ml of 75% strength methanol, again filtered off and dried in vacuo. 2-Azido-5-chloro-benzophenone-oxime of melting point 125°-132°C is obtained. A sample of the crude product is recrystallised from benzene/cyclohexane, after which the pure compound melts at 135°-137°C.

Aufarbeitung

  1. temperatureunder reflux
  2. customevaporated in vacuo at 60°C
  3. additionthe solution is poured into 250 ml of 2 N hydrochloric acid
  4. customThe crude product which precipitates
  5. filtrationis filtered off
  6. filtrationagain filtered off
  7. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-f5d77adaa3f142299a07907044b24b7d
Quelldatensatz
uspto-grants-1976_03
Patentnummer
US03943145

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