反应详情

Iodine (2.14 g, manufactured by Kanto Chemical Co., Inc.) and potassium hydroxide (475 mg, manufactured by Wako Pure Chemical Industries, Ltd.) were added to a solution of 6-nitro-1H-indazole (690 mg, manufactured by Wako Pure Chemical Industries, Ltd.) in N,N-dimethylformamide (20 mL, manufactured by Kanto Chemical Co., Inc.), and the mixture was stirred for one hour at room temperature. A saturated aqueous solution of sodium thiosulfate (20 mL) was added to the reaction solution, and the mixture was extracted with chloroform (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 (chloroform:methanol=9:1), to give 1.04 g of the title compound. LC-MS: HPLC retention time 0.54 minutes, m/z 290 (M+H), condition C-3.

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