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

HRID 1081387ノート

反応式

HRID 1081387 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-fbc2a323404447228743f7da6d7b363f
出典データセット
uspto-grants-1996_12
特許番号
US05585493

反応ノート

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