反应详情

A solution of 240 mg (0.543 mmol) 5-(4,5-diiodo-2-methyl-imidazol-1-yl)-2-methyl-2H-pyridazin-3-one in 17 ml of dry THF was cooled to −78° C. and 0.41 ml of a 1.6M solution of n-butyllithium (0.65 mmol) in hexane was added. The mixture was stirred for 5 min., quenched by addition of 0.5 ml of methanol and stirred for an additional 10 min at −78° C. Then 2 ml of saturated ammonium chloride solution was added and the mixture was allowed to warm up to room temperature. After standard workup with ethyl acetate/water, the crude material was purified by flash chromatography on silicagel using a 90:10 mixture of ethyl acetate/heptane as eluant to yield 53 mg (0.168 mmol, 31%) of the title compound as a light yellow solid, MS: m/e=316.9 (M+H+).

1. customquenched by addition of 0.5 ml of methanol
2. stirringstirred for an additional 10 min at −78° C
3. additionThen 2 ml of saturated ammonium chloride solution was added
4. customAfter standard workup with ethyl acetate/water, the crude material was purified by flash chromatography on silicagel
5. additiona 90:10 mixture of ethyl acetate/heptane as eluant