反应详情

The product of step (a) above (6.3 g), iron powder (6.3 g) and ammonium chloride (6.3 g) were stirred together with ethanol (63 ml) and water (120 ml) and heated under reflux for 1 hour. The hot mixture was filtered and the residue washed with hot ethyl acetate (500 ml). The combined filtrates were separated and the aqueous phase extracted with ethyl acetate. The combined ethyl acetate extracts were washed with water and brine, then dried and evaporated to leave a foam. Upon trituration with ether the sub-title compound was formed as a grey solid, MS MW bp 331.

1. temperatureheated
2. temperatureunder reflux for 1 hour
3. filtrationThe hot mixture was filtered
4. washthe residue washed with hot ethyl acetate (500 ml)
5. customThe combined filtrates were separated
6. extractionthe aqueous phase extracted with ethyl acetate
7. washThe combined ethyl acetate extracts were washed with water and brine
8. customdried
9. customevaporated
10. customto leave a foam