Hydrochloric Acid → 4-Cyano-4'-trifluoromethylbutyrophenone O-(2-aminoethyl) oxime hydrochloride

HRID 2083394Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2083394
[C:1]([CH2:3][CH2:4][CH2:5][C:6]([C:8]1[CH:13]=[CH:12][C:11]([C:14]([F:17])([F:16])[F:15])=[CH:10][CH:9]=1)=O)#[N:2].[ClH:18].Cl.[NH2:20][O:21][CH2:22][CH2:23][NH2:24].N1C=CC=CC=1.Cl>C(O)C>[ClH:18].[NH2:24][CH2:23][CH2:22][O:21][N:20]=[C:6]([C:8]1[CH:13]=[CH:12][C:11]([C:14]([F:17])([F:16])[F:15])=[CH:10][CH:9]=1)[CH2:5][CH2:4][CH2:3][C:1]#[N:2]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 143623262-(O-aminooxy)ethylamine dihydrochlorideHCID 203585325-Oxo-5-(4-trifluoromethylphenyl)valeronitrile

Produkt 1

HCID 867356254-Cyano-4'-trifluoromethylbutyrophenone O-(2-aminoethyl) oxime hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

5.6 Mmol (1.35 g) of 4-cyano-4'-trifluoromethylbutyrophenone, 5.6 mmol (0.84 g) of 2 aminooxyethylamine dihydrochloride and 0.8 ml of pyridine were refluxed in 20 ml of absolute ethanol for 2.5 hours. The processing was equal to that of example 1. The resulting free base was dissolved in absolute ethanol and an equivalent quantity of 2N alcoholic hydrochloric acid was added. The ethanol was then removed in vacuo and the residue was crystallized twice from ethanol/ether (1:5). The melting point of the resulting title compound was 136°-136.5° C.

Aufarbeitung

  1. customThe ethanol was then removed in vacuo
  2. customthe residue was crystallized twice from ethanol/ether (1:5)
  3. customwas 136°-136.5° C.

Quellen und Nachweise

ORD-Eintrag
ord-cd98fd0404eb4f61809f5482a0c88104
Quelldatensatz
uspto-grants-1978_04
Patentnummer
US04085225

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