反应详情

Over a solution of 6-fluorotetralone (6-fluoro-3,4-dihydro-1H-naphthalen-2-one; 1 equivalent) and ammonium acetate (5 equivalents) in a 2:1 mixture of MeOH:THF (0.24 M), was carefully added NaCNBH3 (2 eq), and the reaction mixture was stirred at room temperature for 2 hours. Concentrated HCl was added at 0° C. until the pH was less than 2, and the MeOH was removed in vacuo. The residue was taken up in water and extracted with CHCl3 (2×). The aqueous solution was basified with solid KOH and extracted with CHCl3 (3×). The combined extracts were dried (MgSO4) and evaporated in vacuo to give the titled compound.

1. customthe MeOH was removed in vacuo
2. extractionextracted with CHCl3 (2×)
3. extractionextracted with CHCl3 (3×)
4. dry with materialThe combined extracts were dried (MgSO4)
5. customevaporated in vacuo