تفاعل #86798
ord-32029e594183455090636c28c41dfcdc
معادلة التفاعل
الكواشف
لا شيء
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1استخلاصThe aqueous were extracted with dichloromethane
- 2أخرىthe organic layers rejoined were dried
- 3تركيزconcentrated under reduced pressure
- 4أخرىthe crude material was purified by flash chromatography on silica gel (eluent 2 to 20% ethyl acetate in heptane)
الإجراء التجريبي
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%).