Sodium Hydroxide → 3,4-Dichloro-N'-hydroxybenzene-1-carboximidamide

HRID 880030ノート

反応式

HRID 880030 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[Cl:10])[C:5]#[N:6].Cl.[NH2:12][OH:13].[OH-].[Na+]>C(O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[Cl:10])/[C:5](=[N:12]/[OH:13])/[NH2:6]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 810513,4-DichlorobenzonitrileHCID 443297Hydroxyamine hydrochloride

生成物 1

HCID 112641853,4-Dichloro-N'-hydroxybenzene-1-carboximidamide

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 3,4-dichlorobenzonitrile (2.000 g, 11.63 mmol), hydroxylamine hydrochloride (1.649 mL, 12.79 mmol) and sodium hydroxide (4.15 mL, 12.4 mmol) in ethanol (40 mL) was stirred at rt for 1 h. Concentrated and refluxed in hexane for 30 min and concentrated in vacuo. The product Intermediate 1A was used directly for the next step. HPLC/MS (Method C) RT=1.24 min [M+H]+ 204.9.

後処理

  1. concentrationConcentrated
  2. temperaturerefluxed in hexane for 30 min
  3. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-7f9a9f93621a4f90b113d384f20d4f43
出典データセット
uspto-grants-2015_03
特許番号
US08993557B2

反応ノート

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