反应详情

To a solution of [4-(4-benzyl-morpholin-2-yl)-phenyl]-(2,6-dichloro-phenyl)-amine (0.72 g; 1.74 mmol) in 1,2-dichloroethane (5 mL) was added, drop wise, ACE-Cl (0.40 mL; 3.66 mmol) at 0° C. The resulting mixture was stirred at room temperature, overnight, and subsequently concentrated in vacuo. To the residue was added toluene and the mixture was concentrated in vacuo. This last step was repeated twice. To the final residue was added MeOH (5 mL), and this mixture was stirred overnight at RT. Once more the mixture was concentrated in vacuo. The residue was partitioned between EtOAc and 2 M Aqueous NaOH. The layers were separated, and the organic layer dried (Na2SO4), filtered, and concentrated in vacuo to afford (2,6-dichloro-phenyl)-(4-morpholin-2-yl-phenyl)-amine (0.34 g); which was used as such.

1. customat 0° C
2. concentrationsubsequently concentrated in vacuo
3. additionTo the residue was added toluene
4. concentrationthe mixture was concentrated in vacuo
5. additionTo the final residue was added MeOH (5 mL)
6. stirringthis mixture was stirred overnight at RT
7. concentrationOnce more the mixture was concentrated in vacuo
8. customThe residue was partitioned between EtOAc and 2 M Aqueous NaOH
9. customThe layers were separated
10. dry with materialthe organic layer dried (Na2SO4)
11. filtrationfiltered
12. concentrationconcentrated in vacuo