反应详情

温度

50 °C

A mixture of 1.21 g of 2-butyl -5-cyano-4-(1-hydroxy-1-methyl propyl)-1-tritylimidazole (prepared as described in Preparation 17) and 20 ml of 75% v/v aqueous acetic acid was stirred at 50° C. for 1 hour, after which the mixture was cooled, and the deposited crystals of trityl alcohol were removed by filtration. The filtrate was concentrated by evaporation under reduced pressure, and the remaining water and acetic acid were distilled off as a toluene azeotrope under reduced pressure. The residue was purified by column chromatography through silica gel, using a 9:1 by volume mixture of methylene chloride and methanol as the eluent, to give 0.47 g of the title compound as a crystalline powder, melting at 139°-142° C.

1. temperatureafter which the mixture was cooled
2. customthe deposited crystals of trityl alcohol were removed by filtration
3. concentrationThe filtrate was concentrated by evaporation under reduced pressure
4. distillationthe remaining water and acetic acid were distilled off as a toluene azeotrope under reduced pressure
5. customThe residue was purified by column chromatography through silica gel
6. additionby volume mixture of methylene chloride and methanol as the eluent