Sulfuric Acid → HCID 18917664, compound

Participants

Reaction Conditions

Reaction Steps

6-Phenyl-1-undecyl-4H-[1,2,4]triazolo[4,3-a][1,4]benzodiazepine diazepine (3.2 g) obtained in Example 19 was dissolved in dioxane (30 ml). Thereto were added water (30 ml) and sulfuric acid (2.1 ml) and the mixture was stirred at 60° C. for 1 hour. Thereto was gradually added dropwise a solution of sodium nitrite (5.5 g) in water (20 ml) and the mixture was stirred at 70° C. for 2 hours. After cooling, potassium carbonate was added thereto to make the reaction mixture alkaline. The mixture was extracted with ethyl acetate, washed with water and dried over anhydrous magnesium sulfate. After filtration, the filtrate was concentrated under reduced pressure and the residue was purified by silica gel column chromatography to give 0.4 g of 2-(3-hydroxymethyl-5-undecyl-1,2,4-triazol-4-yl)benzophenone as an oily substance, melting point 111°-112° C.

Provenance & Evidence