反应详情

A suspension of the compound obtained in Step D (42.02 mmoles) in a mixture of EtOH (350 ml) and acetic acid (26 ml) is heated at reflux for 5 minutes. Powdered iron (309 mmoles) and FeCl3.6H2O (2.1 mmoles) are added to the resulting solution. The reaction mixture is stirred at reflux overnight. After evaporation, water (250 ml) is added to the residue and then sonicated for 2 minutes. The mixture is made alkaline (pH 12) using aqueous 2M sodium hydroxide solution, then diluted with AcOEt (500 ml) and then filtered over Celite. The phases are separated and the aqueous phase is extracted with AcOEt. The organic phases are combined. The organic phase obtained is washed with water and then with saturated NaCl solution, dried over sodium sulphate, filtered and evaporated to dryness. The residue is triturated in ethyl ether, filtered and dried in vacuo to yield the title product in the form of a white powder, which is used directly in the next Step.

1. temperatureis heated
2. temperatureat reflux for 5 minutes
3. temperatureat reflux overnight
4. customAfter evaporation, water (250 ml)
5. additionis added to the residue
6. customsonicated for 2 minutes
7. additiondiluted with AcOEt (500 ml)
8. filtrationfiltered over Celite
9. customThe phases are separated
10. extractionthe aqueous phase is extracted with AcOEt
11. customThe organic phase obtained
12. washis washed with water
13. dry with materialwith saturated NaCl solution, dried over sodium sulphate
14. filtrationfiltered
15. customevaporated to dryness
16. customThe residue is triturated in ethyl ether
17. filtrationfiltered
18. customdried in vacuo