Acetone → HCID 11118528、化合物

HRID 1756744ノート

反応式

HRID 1756744 の反応式
[CH3:1][C:2]1[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][C:3]=1[O:4][CH2:5][C:6]1[CH:13]=[CH:12][CH:11]=[CH:10][C:7]=1[CH2:8]Cl.[C-:19]#[N:20].[Na+].CC(C)=O>[Cl-].C([N+](CC)(CC)CC1C=CC=CC=1)C.O>[CH3:1][C:2]1[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][C:3]=1[O:4][CH2:5][C:6]1[CH:13]=[CH:12][CH:11]=[CH:10][C:7]=1[CH2:8][C:19]#[N:20]

参加物

6

反応物 3

HCID 180AcetoneHCID 8929Sodium CyanideHCID 10879843HCID 10879843、化合物

生成物 1

HCID 11118528HCID 11118528、化合物収率 97.9%

試薬・触媒・溶媒 2

HCID 66133Benzyl triethylammonium chloride触媒HCID 962Water溶媒2 回

実験手順

2-(2,5-Dimethylphenoxymethyl)benzyl chloride (Purity: 86.8%, 1.50 g, 5 mmol), 95% sodium cyanide (0.31 g, 6 mmol), triethylbenzylammonium chloride (0.06 g, 0.25 mmol), acetone (4 ml) and water (2 ml) were added. The mixture was heated under reflux for 5 hours. After completion of the reaction, water (100 ml) was added. The resulting mixture was extracted with ether (100 ml), dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (ethyl acetate/n-hexane) to give 2-(2,5-dimethylphenoxymethyl)benzyl cyanide (1.23 g, Yield: 97.8%).

後処理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 5 hours
  3. additionwas added
  4. extractionThe resulting mixture was extracted with ether (100 ml)
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe resulting residue was purified by silica gel chromatography (ethyl acetate/n-hexane)

出典と根拠

ORDレコード
ord-ece814a5ade64485aab6f64bfc021c3f
出典データセット
uspto-grants-1995_08
特許番号
US05442063

反応ノート

読み込み中…