反应详情

252 mg of 4-Chloro-benzoic acid N′-[2-(2,6-dimethyl-4-morpholin-4-yl-phenyl)-3H-benzoimidazole-5-carbonyl]-hydrazide was placed in a microwave tube and dissolved in 4 ml of THF. 300 mg of (methoxycarbonylsulfamoyl)triethylammonium hydroxide (Burgess Reagent) was added and the tube was sealed and microwaved at 150° C. for 30 minutes. The reaction was then diluted with water and heptane. The precipitates were collected by filtration and purified by column chromatography (heptane:ethyl acetate=1:1 to 1:2) to provide the title compound. LCMS ret T=1.44 min, m/z=486.1, method 10. 1H NMR (400 MHz, MeOD) □ ppm 2.29 (br. s., 6 H) 3.36 (br. s., 5 H) 3.99 (br. s., 4 H) 6.95 (br. s., 2 H) 7.81 (s, 2 H) 7.95 (br. s., 1 H) 8.25 (br. s., 1 H) 8.32 (br. s., 2 H) 8.56 (br. s., 1 H).

1. customthe tube was sealed
2. custommicrowaved at 150° C. for 30 minutes
3. filtrationThe precipitates were collected by filtration
4. custompurified by column chromatography (heptane:ethyl acetate=1:1 to 1:2)