Acetyl chloride → HCID 10845679、化合物
反応式
[C:1](Cl)(=O)[CH3:2].[CH2:5]([O:7][C:8]1[C:12]([CH3:13])=[C:11]([C:14]([OH:16])=[O:15])[O:10][N:9]=1)[CH3:6].C([O-])(O)=O.[Na+]>CCO>[CH2:5]([O:7][C:8]1[C:12]([CH3:13])=[C:11]([C:14]([O:16][CH2:1][CH3:2])=[O:15])[O:10][N:9]=1)[CH3:6]参加物
5
反応条件
- 温度
- 0 °C
実験手順
Acetyl chloride (25 mL, 0.35 mol) was added to EtOH (250 mL) at 0° C. and the solution was stirred at 0° C. for 20 min. A solution of 3-ethoxy-4-methylisoxazole-5-carboxylic acid (WO95/12587,A1) (18 g, 0.10 mol) in EtOH (20 ml) was added and the resulting mixture was boiled under reflux for 4 h. The mixture was cooled, added NaHCO3 (200 mL) and extracted with diethylether (3×300 mL). The organic extracts were dried (MgSO4) and concentrated in vacuo to afford crude title compound (18 g, 86%).
後処理
- temperatureunder reflux for 4 h
- temperatureThe mixture was cooled
- extractionextracted with diethylether (3×300 mL)
- dry with materialThe organic extracts were dried (MgSO4)
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-d7bd94f6375342e1a3b9550d0889f586
- 出典データセット
- uspto-grants-2001_03
- 特許番号
- US06200999B1
反応ノート
読み込み中…