反应详情

A solution of 108 mg of sodium borohydride in 20 ml of ethanol was added to a solution of 2.00 g of 2-propyl -4-pivaloyl-1-[4-[2-(trityltetrazol-5-yl)-phenyl]phenyl}methylimidazole-5-carbonitrile [prepared as described in step (a) above] in 40 ml of tetrahydrofuran, and the mixture was stirred at room temperature for 2.5 hours. An the end of this time, the reaction mixture was concentrated by evaporation under reduced pressure, and the residue was dissolved in a mixture of ethyl acetate and water. The ethyl acetate layer was separated, washed with water, dried over anhydrous magnesium sulfate and concentrated by evaporation under reduced pressure. The syrupy residue was crystallized in a 1:4 by volume mixture of ethyl acetate and hexane, to give 1.93 g of the title compound as crystals, melting at 115°-117° C.

1. concentrationAn the end of this time, the reaction mixture was concentrated by evaporation under reduced pressure
2. dissolutionthe residue was dissolved in a mixture of ethyl acetate and water
3. customThe ethyl acetate layer was separated
4. washwashed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated by evaporation under reduced pressure
7. customThe syrupy residue was crystallized in a 1:4 by volume mixture of ethyl acetate and hexane