Hydrochloric Acid → N-[2,2,2-Trifluoro-1-(4-methoxyphenyl)ethylidene]hydroxylamine

HRID 1384779

反応式

HRID 1384779 の反応式
[F:1][C:2]([F:20])([F:19])[C:3]([C:6]1[CH:11]=[CH:10][C:9]([O:12][C:13]2C=CC=CC=2)=[CH:8][CH:7]=1)=[N:4][OH:5].Cl>C(Cl)Cl>[F:1][C:2]([F:19])([F:20])[C:3]([C:6]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[CH:8][CH:7]=1)=[N:4][OH:5]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 59115193HCID 59115193、化合物2 回

生成物 1

HCID 59115151N-[2,2,2-Trifluoro-1-(4-methoxyphenyl)ethylidene]hydroxylamine収率 122.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2,2,2-Trifluoro-1-(4-phenoxyphenyl)-ethanone oxime (single isomer) 35 g (124 mmol) of 2,2,2-trifluoro-1-(4-phenoxyphenyl)-ethanone oxime (mixture of E- and Z-isomers) prepared according to the method described in example 80.1 is dissolved in 300 ml of methylene chloride. To the solution is added 1.1 ml of conc. HCl and stirred at room temperature for 4.5 hours. The reaction mixture is washed with water and brine, dried over MgSO4, and concentrated, yielding 33.4 g of 2,2,2-trifluoro-1-(4-methoxyphenyl)-ethanone oxime (single isomer) as a white solid. The structure is confirmed by the 1H-NMR spectrum (CDCl3). δ[ppm]: 7.00-7.12 (m, 4H), 7.19 (t, 1H), 7.39 (t, 2H), 7.57 (d, 2H), 8.95 (s, 1H).

後処理

  1. washThe reaction mixture is washed with water and brine
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-ad3fc87af70f493aa3ad56fb90d74dc7
出典データセット
uspto-grants-2001_07
特許番号
US06261738B1

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