2-Iodoxybenzoic acid → HCID 67131087、化合物
反応式
I(C1C=CC=CC=1C(O)=O)(=O)=O.[Cl:13][C:14]1[CH:19]=[CH:18][C:17]([N:20]2[C:28]([CH:29]([CH:31]3[CH2:36][CH2:35][CH2:34][CH2:33][CH2:32]3)[OH:30])=[C:27]3[C:22]([CH:23]=[CH:24][CH:25]=[CH:26]3)=[N:21]2)=[CH:16][CH:15]=1>C1COCC1.CS(C)=O>[Cl:13][C:14]1[CH:19]=[CH:18][C:17]([N:20]2[C:28]([C:29]([CH:31]3[CH2:32][CH2:33][CH2:34][CH2:35][CH2:36]3)=[O:30])=[C:27]3[C:22]([CH:23]=[CH:24][CH:25]=[CH:26]3)=[N:21]2)=[CH:16][CH:15]=1参加物
4
実験手順
2-Iodoxybenzoic acid (1.42 g, 2.3 mmol; 45% purity) was added to an ice cold solution of [2-(4-chloro-phenyl)-2H-indazol-3-yl]-cyclohexyl-methanol (520 mg, 1.5 mmol) in THF/DMSO 1/1 (28 ml). The reaction mixture was stirred for 1 h at ambient temperature, ice water/brine 1/1 was added and the mixture was extracted two times with iPrOAc. The combined extracts were washed with ice water/saturated aqueous ammonium chloride solution 1/1 and dried over Na2SO4. After filtration the solvent was removed under reduced pressure and the residue was purified by column chromatography (silica gel, iPrOAc/heptane) to give the title compound (404 mg, 1.2 μmol; 78%) as colorless solid. MS: m/e=339.1 [M+H+].