反应详情

Potassium hydroxide (73 mg, manufactured by Wako Pure Chemical Industries, Ltd.) and iodine (330 mg, manufactured by Kanto Chemical Co., Inc.) were added to a solution of 6-(trifluoromethyl)-1H-indazole (121 mg) synthesized according to the literature (Shoji, et al., Tetrahedron Lett., 2004, 45, 1769-1772) in N,N-dimethylformamide (6.5 mL, manufactured by Kanto Chemical Co., Inc.), and the mixture was stirred for 3 hours at room temperature. An aqueous solution of sodium thiosulfate (20 mL) was added to the reaction solution, and the mixture was extracted with ethyl acetate (3×20 mL), washed with brine (40 mL), and dried (MgSO4). The solvent was then evaporated. The resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1), to give 169 mg of the title compound. LC-MS: HPLC retention time 4.46 minutes, m/z 313 (M+H), condition B-1.

1. customsynthesized
2. extractionthe mixture was extracted with ethyl acetate (3×20 mL)
3. washwashed with brine (40 mL)
4. dry with materialdried (MgSO4)
5. customThe solvent was then evaporated
6. customThe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1)