Ethanol → [(E)-3-[4-chloro-3-(trifluoromethyl)phenyl]prop-2-enoyl]-oxidoazanium

HRID 1491971ノート

反応式

HRID 1491971 の反応式
[Cl:1][C:2]1[CH:11]=[CH:10][C:5]([CH:6]=[CH:7]C#N)=[CH:4][C:3]=1[C:12]([F:15])([F:14])[F:13].Cl.[NH2:17][OH:18].[C:19](=[O:22])([O-])[O-].[Na+].[Na+].C(O)C>O>[Cl:1][C:2]1[CH:11]=[CH:10][C:5](/[CH:6]=[CH:7]/[C:19]([NH2:17]=[O:18])=[O:22])=[CH:4][C:3]=1[C:12]([F:15])([F:14])[F:13]

参加物

6

反応物 4

HCID 702EthanolHCID 10340Sodium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 541762263-[4-Chloro-3-(trifluoromethyl)phenyl]prop-2-enenitrile

生成物 1

HCID 23364570[(E)-3-[4-chloro-3-(trifluoromethyl)phenyl]prop-2-enoyl]-oxidoazanium収率 39.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

12.1 g (0.05 mol) of 4-chloro-3-trifluoromethyl-cinnamonitrile are added to a solution of 7.2 g (0.10 mol) of hydroxylamine hydrochloride, 7.3 g (0.10 mol) of sodium carbonate in 100 ml of water, and 100 ml of ethanol. The mixture is refluxed until the reaction is complete (24 hours) and the entire batch is subsequently stirred into 250 ml of water. The solid which separates out during this process is filtered off with suction, washed with a little water and dried. 5.3 g (39.3% of theory) of (E)-4-chloro-3-trifluoromethyl-cinnamamide oxide are obtained.

後処理

  1. temperatureThe mixture is refluxed until the reaction
  2. custom(24 hours)
  3. filtrationis filtered off with suction
  4. washwashed with a little water
  5. customdried

出典と根拠

ORDレコード
ord-068deb44a5de4ac58aed5685f015a7f9
出典データセット
uspto-grants-1994_12
特許番号
US05371231

反応ノート

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