反应详情

A solution of the product of part (ii) (10.0 g) in ethanol (400 ml) and 2N hydrochloric acid (200 ml) was heated to reflux with stirring. Zinc dust (8.80 g) was added at such a rate that the ensuing reaction was not too vigorous. The mixture was heated under reflux for 0.25 hour and then cooled and filtered. The filtrate was made basic with 0.88 ammonia solution and diluted with a large volume of water. The mixture was extracted several times with ethyl acetate and the combined extracts were washed with water and dried (Na2SO4). Evaporation of the solvent gave an oil which was chromatographed on silica gel, eluting with dichloromethane. Earlier fractions contained impurity and the pure product was eluted in the later fractions. The product fractions were combined and evaporated to give an oil, (5.50 g). The product darkened rapidly and was used directly without further purification.

1. temperatureto reflux
2. customthat the ensuing reaction
3. temperatureThe mixture was heated
4. temperatureunder reflux for 0.25 hour
5. temperaturecooled
6. filtrationfiltered
7. additiondiluted with a large volume of water
8. extractionThe mixture was extracted several times with ethyl acetate
9. washthe combined extracts were washed with water
10. dry with materialdried (Na2SO4)
11. customEvaporation of the solvent
12. customgave an oil which
13. customwas chromatographed on silica gel
14. washeluting with dichloromethane
15. washthe pure product was eluted in the later fractions
16. customevaporated
17. customto give an oil, (5.50 g)
18. customwas used directly without further purification