反应详情

To a THF (10 mL) solution of 2-(2-fluoro-4-{2-[4-(trifluoromethyl)phenoxy]-ethyl}phenyl)-1,3-dioxolane (0.552 g) was added 6 M HCl (0.775 mL) at 0° C., then the resultant mixture was room temperature for 5 hours. The reaction mixture was evaporated to afford a pale yellow oil. To a CH2Cl2 (15 mL) solution of that pale yellow oil and tert-Butyl 1-piperazinecarboxylate (0.375 g) were added NaB(OAc)3 (0.657 g) at 0° C. The resultant mixture was stirred at room temperature for 3 days. To the reaction mixture was added saturated aqueous NaHCO3, and extracted with CH2Cl2. The organic layer was washed with saturated aqueous NaCl, dried over anhydrous MgSO4, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (n-hexane/AcOEt=9/1 to 4/1) to afford tert-butyl 4-(2-fluoro-4-{2-[4-(trifluoromethyl)phenoxy]ethyl}benzyl)piperazine-1-carboxylate as a colorless oil (0.511 g).

1. customThe reaction mixture was evaporated
2. customto afford a pale yellow oil
3. extractionextracted with CH2Cl2
4. washThe organic layer was washed with saturated aqueous NaCl
5. dry with materialdried over anhydrous MgSO4
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by silica gel column chromatography (n-hexane/AcOEt=9/1 to 4/1)