Potassium Hydroxide → 5-(Chloromethyl)-1,2-oxazole-3-carboxylic acid
反応式
[Cl:1][CH2:2][C:3]1[O:7][N:6]=[C:5]([C:8]([O:10]CC)=[O:9])[CH:4]=1.[OH-].[K+]>C(O)C>[Cl:1][CH2:2][C:3]1[O:7][N:6]=[C:5]([C:8]([OH:10])=[O:9])[CH:4]=1参加物
4
反応条件
- 温度
- 65 °C
実験手順
47.3 g (250 mmol) of ethyl 5-chloromethylisoxazole-3-carboxylate in 150 ml of ethanol were mixed with 14 g (250 mmol) of potassium hydroxide, and the mixture was stirred at 60-70° C. for 6 h. After cooling and concentration under reduced pressure, the residue was taken up in water and extracted with ether, the aqueous phase was acidified with hydrochloric acid and then extracted several times with ether, and the ether phase was dried over sodium sulfate and concentrated under reduced pressure (oil pump, 50° C.). 31 g of the required product were obtained (77% of theory).
後処理
- temperatureAfter cooling
- concentrationconcentration under reduced pressure
- extractionextracted with ether
- extractionextracted several times with ether
- dry with materialthe ether phase was dried over sodium sulfate
- concentrationconcentrated under reduced pressure (oil pump, 50° C.)
出典と根拠
- ORDレコード
- ord-f240dec859874514930a0cecc8b078e3
- 出典データセット
- uspto-grants-2000_09
- 特許番号
- US06114358
反応ノート
読み込み中…