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

HRID 2083394ノート

反応式

HRID 2083394 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-cd98fd0404eb4f61809f5482a0c88104
出典データセット
uspto-grants-1978_04
特許番号
US04085225

反応ノート

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