反应详情

A portion of solid (4-{4-methyl-5-[2-(trifluoromethyl)phenyl]-4H-1,2,4-triazol-3-yl}bicyclo[2.2.2]octane-1-carboxylic acid 1-D (2.0 g, 5.27 mmol) was dissolved in anhydrous DMF (30 ml) and treated with N,N,N′,N′-tetramethylformamidinium hexafluorophosphate (2.09 g, 7.91 mmol), triethyl amine (2.3 mL, 16.50 mmol), and hydrazine (0.50 mL, 15.93 mmol) at room temperature and a nitrogen atmosphere overnight. The solvent was removed in vacuo, and the residue was redissolved in methylene chloride (700 ml) and washed with saturated aqueous sodium bicarbonate, water, and brine. The product was dried over MgSO4 and the solvent removed to afford 13-A as a white powder. MS (ESI+)=394.13 (M+1).

1. customa nitrogen atmosphere overnight
2. customThe solvent was removed in vacuo
3. dissolutionthe residue was redissolved in methylene chloride (700 ml)
4. washwashed with saturated aqueous sodium bicarbonate, water, and brine
5. dry with materialThe product was dried over MgSO4
6. customthe solvent removed