反应详情

A suspension of silver carbonate (560 mg), 2,6-dichloro-4-nitrobenzylchloride (440 mg) in 2-methoxyethanol (9 cm3) and water (9 cm3) were heated at reflux for 18 h. After this time the hot reaction mixture was filtered and the filtrate diluted with dichloromethane (30 cm3) and water (20 cm3). The heterogeneous mixture was shaken, separated and the aqueous phase extracted with dichloromethane (30 cm3). Combined organic extracts were washed with saturated brine, dried and evaporated to leave an orange oil which was purified by chromatography over silica gel with an ethyl acetate--petroleum ether gradient. The title compound was obtained as a cream solid, m.p. 111°-114° C.

1. temperaturewere heated
2. temperatureat reflux for 18 h
3. filtrationAfter this time the hot reaction mixture was filtered
4. additionthe filtrate diluted with dichloromethane (30 cm3) and water (20 cm3)
5. customseparated
6. extractionthe aqueous phase extracted with dichloromethane (30 cm3)
7. washCombined organic extracts were washed with saturated brine
8. customdried
9. customevaporated
10. customto leave an orange oil which
11. customwas purified by chromatography over silica gel with an ethyl acetate