Hydroxylamine HCl → 2-Chloro-3-hydroxybenzonitrile

HRID 222338

反応式

HRID 222338 の反応式
[Cl:1][C:2]1[C:9]([OH:10])=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=O.[Cl-].O[NH3+:13]>C(O)(=O)C.C(OCC)(=O)C>[Cl:1][C:2]1[C:9]([OH:10])=[CH:8][CH:7]=[CH:6][C:3]=1[C:4]#[N:13]

参加物

5

反応物 2

HCID 21645Hydroxylamine HClHCID 5933762-Chloro-3-hydroxybenzaldehyde

生成物 1

HCID 214365452-Chloro-3-hydroxybenzonitrile

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 2-chloro-3-hydroxybenzaldehyde [(2 g, 12.8 mmol) WO 2005007633, p 34] and hydroxylammonium chloride (1.33 g, 19.6 mmol) in acetic acid (20 mL) was heated under reflux for 2 hours. The reaction mixture was then cooled to room temperature and partitioned between diethyl ether and water. The organic layer was separated, washed with brine, dried over magnesium sulfate and concentrated in vacuo to give a white solid. The solid was then dissolved in ethyl acetate washed with water and brine, dried over magnesium sulfate and concentrated in vacuo to afford the title compound as a solid in quantitative yield.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 2 hours
  3. custompartitioned between diethyl ether and water
  4. customThe organic layer was separated
  5. washwashed with brine
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated in vacuo
  8. customto give a white solid
  9. washwashed with water and brine
  10. dry with materialdried over magnesium sulfate
  11. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-3228a409c4a9446ebecc30f3b3fc2962
出典データセット
uspto-grants-2012_06
特許番号
US08207198B2

関連ノート

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