反应详情

A mixture of the product from step (iv) (9.51 g) and pentylamine (12 ml) in dioxane (100 ml) was heated under reflux for 48 h. The solvent was evaporated and the residue partitioned between EtOAc/water. The organics were separated, washed with aq NaHCO3 soln, water, dried and evaporated under reduced pressure. The residue was dissolved in MeOH (200 ml) then aq NaOH (2M, 40 ml) added and the mixture heated under reflux for 6 h. The mixture was acidified to pH 7 with aq 2M HCl, the solvent evaporated under reduced pressure and the residue partitioned between DCM/water. The organics were separated, washed with aq NaHCO3 soln, brine, dried and evaporated under reduced pressure. The residue was triturated with ethyl acetate and filtered to afford the subtitle compound, 2.43 g.

1. temperaturewas heated
2. temperatureunder reflux for 48 h
3. customThe solvent was evaporated
4. customthe residue partitioned between EtOAc/water
5. customThe organics were separated
6. washwashed with aq NaHCO3 soln
7. dry with materialwater, dried
8. customevaporated under reduced pressure
9. dissolutionThe residue was dissolved in MeOH (200 ml)
10. additionaq NaOH (2M, 40 ml) added
11. temperaturethe mixture heated
12. temperatureunder reflux for 6 h
13. customthe solvent evaporated under reduced pressure
14. customthe residue partitioned between DCM/water
15. customThe organics were separated
16. washwashed with aq NaHCO3 soln
17. dry with materialbrine, dried
18. customevaporated under reduced pressure
19. customThe residue was triturated with ethyl acetate
20. filtrationfiltered