反应详情

A solution of 2-(4-chlorobutyl)-2,4-dihydro-1H-[1,2,4]triazolo[3,4-c][1,4]benzoxazin-1-one, (1.40 g., 0.005 mole), potassium iodide (0.83 g.; 0.005 mole) and 4-(2-keto-1-benzimidazolinyl)piperidine (2.39 g.; 0.011 mole) in 25 ml. of DMF was warmed to 115° C. and stirred for 4.75 hours. The resulting solution was cooled, poured into saturated sodium bicarbonate aqueous solution and extracted with methylene chloride. The methylene chloride extracts were combined and washed with brine solution, dried over sodium sulfate and concentrated in vacuo. The resulting residue was crystallized from ethyl acetate to give 1.87 g., m.p. 173°-175.5° C. and 0.03 g., m.p. 172°-173° C. of the above named end product. The analytical sample had melting point 174°-175.5° C.

1. temperatureThe resulting solution was cooled
2. extractionextracted with methylene chloride
3. washwashed with brine solution
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated in vacuo
6. customThe resulting residue was crystallized from ethyl acetate
7. customto give 1.87 g