反应详情

温度

0 °C

A suspension of lithium aluminum hydride (0.49 g, 12.8 mmol) and THF (5 mL) was cooled to 0° C. and added to a solution of 3-benzyloxy-2,2-dimethyl-1-{4-[2-(2,2,2-trifluoroethoxy)phenyl]piperazin-1-yl}-1-propanone (2.8 g, 6.4 mol) in 12 mL of THF. The mixture was heated 2 hours at reflux, slowly diluted with water, filtered and concentrated. The residue was dissolved in water and the solution was extracted with methylene chloride (4×30 mL). The combined extracts were washed with water (1×25 mL), dried (MgSO4) and concentrated. The residue was purified by chromatography on silica gel eluting with hexanes/ethyl acetate (8:2) to give 3-benzyloxy-2,2-dimethyl-1-{4-[2-(2,2,2-trifluoroethoxy)phenyl]piperazin-1-yl}propane (2.6 g, 6.2 mol).

1. temperatureThe mixture was heated 2 hours
2. temperatureat reflux
3. filtrationfiltered
4. concentrationconcentrated
5. dissolutionThe residue was dissolved in water
6. extractionthe solution was extracted with methylene chloride (4×30 mL)
7. washThe combined extracts were washed with water (1×25 mL)
8. dry with materialdried (MgSO4)
9. concentrationconcentrated
10. customThe residue was purified by chromatography on silica gel eluting with hexanes/ethyl acetate (8:2)