反应详情

To a solution (1000 mL) of 6-[1-hydroxy-2-methyl-1-(1-trityl-1H-imidazol-4-yl)propyl]-N,N-diisopropyl-2-naphthamide (50.0 g) and N,N,N′,N′-tetramethylethylenediamine (94.9 mL) in toluene was added dropwise a butyllithium hexane solution (1.6 M: 196 mL) at −70° C. After stirring at the same temperature for 2 hrs., DMF (60.9 mL) was added dropwise and mixture was stirred for 20 min. Water was added to the reaction solution and the mixture was diluted with ethyl acetate. The organic layer was washed successively with water, 10% aqueous citric acid solution, water and saturated aqueous sodium hydrogen carbonate, and dried over magnesium sulfate. The solvent was evaporated and the obtained residue was recrystallized from hexane-ethyl acetate (3:1) to give the title compound (36.0 g) as a colorless powder.

1. stirringmixture was stirred for 20 min
2. washThe organic layer was washed successively with water, 10% aqueous citric acid solution, water and saturated aqueous sodium hydrogen carbonate
3. dry with materialdried over magnesium sulfate
4. customThe solvent was evaporated
5. customthe obtained residue was recrystallized from hexane-ethyl acetate (3:1)