反应详情

To a solution of 4-benzyl-2-[4-(2,6-dichloro-phenoxymethyl)-phenyl]-morpholine (2.25 g; 3.7 mmol) in 1,2-dichloroethane (10 mL), was added dropwise 1-chloroethyl chloroformate (0.44 mL; 4.0 mmol), at 0° C. After 15 minutes, the cooling was removed and subsequently the mixture was heated under reflux overnight. After cooling to RT the mixture was 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 (10 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-[4-(2,6-Dichloro-phenoxymethyl)-phenyl]-morpholine (0.98 g), which was used as such in the next step.

1. customat 0° C
2. customthe cooling was removed
3. temperaturesubsequently the mixture was heated
4. temperatureunder reflux overnight
5. concentrationwas concentrated in vacuo
6. additionTo the residue was added toluene
7. concentrationthe mixture was concentrated in vacuo
8. additionTo the final residue was added MeOH (10 mL)
9. concentrationOnce more the mixture was concentrated in vacuo
10. customThe residue was partitioned between EtOAc and 2 M Aqueous NaOH
11. customThe layers were separated
12. dry with materialthe organic layer dried (Na2SO4)
13. filtrationfiltered
14. concentrationconcentrated in vacuo