反应详情

Sodium hydride (320 mg, 60% in oil, 7.98 mmol) was washed with iso-hexane (×3) then THF (8 ml) and (1R*,2R*,5R*)-8-benzyl-1-(4-fluorophenyl)-8-azabicyclo[3.2.1]octan-2-ol (Description 15; 1.24 g, 3.99 mmol) added and the mixture stirred at room temperature for 10 minutes then 3,5-bis(trifluoromethyl) benzyl bromide added and the reaction mixture stirred at 60° C. overnight. The reaction mixture was poured into water and extracted with ethyl acetate (×3), dried (MgSO4) and concentrated in vacuo to give a yellow oil. This was purified by flash column chromatography [5% ethyl acetate in iso-hexane] to give the title compound (1.51 g, 58%).

1. stirringthe reaction mixture stirred at 60° C. overnight
2. extractionextracted with ethyl acetate (×3)
3. dry with materialdried (MgSO4)
4. concentrationconcentrated in vacuo
5. customto give a yellow oil
6. customThis was purified by flash column chromatography [5% ethyl acetate in iso-hexane]