Water → Ethyl 5-chloro-1,2-oxazole-3-carboxylate
反応式
C(N([CH2:6][CH3:7])CC)C.Cl[C:9](=[N:15][OH:16])[C:10]([O:12][CH2:13][CH3:14])=[O:11].O.[Cl:18]CCl>ClC(Cl)=C>[Cl:18][C:6]1[O:16][N:15]=[C:9]([C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH:7]=1参加物
6
実験手順
A mixture of triethylamine (13.12 mL; 90.73 mmol) in 1,1-dichloroethene (75 mL) was added to ethyl 2-chloro-2-(hydroxyimino)acetate (5.5 g; 36.29 mmol) in 1,1-dichloroethene (50 mL) over a period of 2 h the reaction mixture was stirred at room temperature for 20 min and portioned between water (75 mL) and dichloromethane (75 mL). The aqueous were extracted with dichloromethane, the organic layers rejoined were dried, concentrated under reduced pressure and the crude material was purified by flash chromatography on silica gel (eluent 2 to 20% ethyl acetate in heptane) to afford ethyl 5-chloroisoxazole-3-carboxylate 2.5 g (39%).
後処理
- extractionThe aqueous were extracted with dichloromethane
- customthe organic layers rejoined were dried
- concentrationconcentrated under reduced pressure
- customthe crude material was purified by flash chromatography on silica gel (eluent 2 to 20% ethyl acetate in heptane)
出典と根拠
- ORDレコード
- ord-32029e594183455090636c28c41dfcdc
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09434722B2
反応ノート
読み込み中…