Water → 4-Acetyl-2-hydroxybenzonitrile
反応式
C([C:4]1[CH:12]=[C:8]([C:9]([NH2:11])=O)[C:7]([OH:13])=[CH:6][CH:5]=1)(=O)C.O=C(Cl)OC(Cl)(Cl)Cl.O.[O:23]1CCO[CH2:25][CH2:24]1>>[OH:13][C:7]1[CH:6]=[C:5]([C:24](=[O:23])[CH3:25])[CH:4]=[CH:12][C:8]=1[C:9]#[N:11]参加物
5
実験手順
5-acetylsalicylamide (10.04 g, 56 mmol) and diphosgene (18.4 g, 93 mmol) were heated in dioxane (65 ml) to70° C. under nitrogen for 18 hours. The mixture was cooled, cautiously poured into cold water (700 ml) and stirred for 1 hour to destroy excess diphosgene reagent. The mixture was extracted with ethyl acetate, and the organic solution washed with water and brine, dried over sodium sulfate, filtered, and evaporated. The residue was recrystallized from toluene/acetonitrile to give the title compound.
後処理
- temperatureThe mixture was cooled
- customto destroy excess diphosgene reagent
- extractionThe mixture was extracted with ethyl acetate
- washthe organic solution washed with water and brine
- dry with materialdried over sodium sulfate
- filtrationfiltered
- customevaporated
- customThe residue was recrystallized from toluene/acetonitrile
出典と根拠
- ORDレコード
- ord-48abb30d71154eea8c58477658514c87
- 出典データセット
- uspto-grants-2003_11
- 特許番号
- US06649636B1
反応ノート
読み込み中…