反应详情

To a solution in a solvent mixture of THF (4.0 mL) and water (1.0 mL) of 2-(trans-4-azidocyclohexyl)-5-phenylbenzimidazole (73.1 mg) as prepared by reacting trans-4-azidocyclohexanecarboxylic acid with 4-phenyl-1,2-phenylenediamine under the same conditions as described in Example 1-3) was added triphenylphosphine (72.0 mg), followed by stirring at room temperature for 1 hr. A portion of the reaction solution was admixed with methanesulfonyl chloride and triethylamine, followed by stirring at the same temperature for 1 hr., and the resultant reaction solution was admixed with conc. aqueous ammonia, followed by concentration under reduced pressure. The residue was separated and purified on a collective thin-layer chromatograph (chloroform:methanol=15:1) to give the title compound.

1. customas prepared
2. stirringby stirring at the same temperature for 1 hr
3. custom, and the resultant reaction solution
4. concentrationfollowed by concentration under reduced pressure
5. customThe residue was separated
6. custompurified on a collective thin-layer chromatograph (chloroform:methanol=15:1)