Potassium Cyanide → 2-(2-Bromo-3-methylphenyl)acetonitrile

HRID 427514

反応式

HRID 427514 の反応式
[Br:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:9]Br.[C-:11]#[N:12].[K+]>CN(C)C=O>[Br:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:9][C:11]#[N:12]

参加物

4

反応条件

温度
90 °C

実験手順

2-bromo-1-(bromomethyl)-3-methylbenzene (15 g, 0.057 mmol) and potassium cyanide (9.6 g, 0. 148 mol) were added to dimethylformamide (75 ml) and stirred at 90° C. overnight. The solvent was evaporated under reduced pressure and the residue partitioned between water (150 ml) and methylene chloride. The aqueous layer was extracted twice with methylene chloride, the organic extracts was separated, washed twice with water and was evaporated under reduced pressure. Purification of the residue by column chromatography on silica gel using heptane:methylene chloride (3:7) as eluent gave 8.0 g (67%) of the title compound.

後処理

  1. customThe solvent was evaporated under reduced pressure
  2. customthe residue partitioned between water (150 ml) and methylene chloride
  3. extractionThe aqueous layer was extracted twice with methylene chloride
  4. customthe organic extracts was separated
  5. washwashed twice with water
  6. customwas evaporated under reduced pressure
  7. customPurification of the residue by column chromatography on silica gel

出典と根拠

ORDレコード
ord-918cb1bb863a44b4bf4df26917291d17
出典データセット
uspto-grants-2001_11
特許番号
US06313137B1

関連ノート

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