Potassium Hydroxide → 5-(Chloromethyl)-1,2-oxazole-3-carboxylic acid
反応式
[OH-].[K+].[Cl:3][CH2:4][C:5]1[O:9][N:8]=[C:7]([C:10]([O:12]CC)=[O:11])[CH:6]=1>C(O)C>[Cl:3][CH2:4][C:5]1[O:9][N:8]=[C:7]([C:10]([OH:12])=[O:11])[CH:6]=1参加物
4
反応条件
- 温度
- 65 °C
実験手順
14 g (250 mmol) of potassium hydroxide were added to 47.3 g (250 mmol) of ethyl 5-chloromethylisoxazole-3-carboxylate in 150 ml of ethanol, and the reaction mixture was stirred for 6 hours at 60-70° C. After cooling, the mixture was concentrated in vacuo, the residue was taken up in water and extracted with ether, the aqueous phase was acidified with hydrochloric acid and subsequently extracted repeatedly with ether, and the ether phase was dried over sodium sulfate and concentrated in vacuo (oil pump, 50° C.). 31 g of the required product resulted (77% of theory)
後処理
- temperatureAfter cooling
- concentrationthe mixture was concentrated in vacuo
- extractionextracted with ether
- extractionsubsequently extracted repeatedly with ether
- dry with materialthe ether phase was dried over sodium sulfate
- concentrationconcentrated in vacuo (oil pump, 50° C.)
出典と根拠
- ORDレコード
- ord-a6726453d7bb47f7847093625a1a8176
- 出典データセット
- uspto-grants-2004_05
- 特許番号
- US06740647B1
反応ノート
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