反应详情

To a solution of the compound obtained in Step B (10.37 mmoles) in ethanol (25 ml) there are added 122 microlitres of acetic acid. The solution is heated at reflux and stirred for 10 minutes. Powdered iron (2.08 g) and 75 mg of FeCl3.6H2O are added. After stirring for 2 hours at reflux, the mixture is brought to ambient temperature and then concentrated to dryness. 50 ml of water are added to the residue obtained, and the pH is made alkaline using sodium hydroxide. The solution is extracted 4 times with AcOEt. The organic phases are combined and washed with saturated aqueous NaCl solution and then dried with MgSO4. After filtration, the organic phase is evaporated to dryness to yield the title product, which is used directly in the next Step.

1. temperatureThe solution is heated
2. temperatureat reflux
3. stirringAfter stirring for 2 hours
4. temperatureat reflux
5. customis brought to ambient temperature
6. concentrationconcentrated to dryness
7. addition50 ml of water are added to the residue
8. customobtained
9. extractionThe solution is extracted 4 times with AcOEt
10. washwashed with saturated aqueous NaCl solution
11. dry with materialdried with MgSO4
12. filtrationAfter filtration
13. customthe organic phase is evaporated to dryness