Water → 1-Cyclohexyl-2-(3,4-diaminophenyl)-1H-benzimidazole-5-carboxylic Acid

関与物質

反応手順

A solution of 1 g (2.84 mmol) of the product of the previous step, 0.91 g (2.84 mmol) of TBTU and 0.73 g (5.68 mmol) of DIEA in 10 mL anhydrous DMF was allowed to stand at room temperature for 15 min. To this solution was added 0.90 g (3.41 mmol) of Compound 11, and the solution was allowed to stand at room temperature overnight. The solution was then poured into 100 mL H2O, stirred for 30 min, filtered and dried. The solution of the solids thus obtained, in 50 mL 1M HCl and 25 mL EtOH, was refluxed at 110° C. overnight. The solvents were removed and the residue was treated with 14 mL 2 M NaOH in 70 mL of MeOH at 60° C. overnight. The MeOH was evaporated, the residue was diluted with 70 mL H2O and acidified to pH 6. The precipitate was filtered, washed with H2O and dried yielding 0.95 g brown solid. MS: 351.20 (M+H+).

情報源と証拠