4-Methoxy-2,6-dimethylbenzene-1-sulfonyl chloride → HCID 178497579、化合物
反応式
[CH3:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[C:4]([CH3:10])[C:3]=1[S:11](Cl)(=[O:13])=[O:12].[CH3:15][NH:16][CH2:17][C:18]1[NH:22][C:21]2[C:23]([C:27]([O:29][CH3:30])=[O:28])=[CH:24][CH:25]=[CH:26][C:20]=2[N:19]=1>C(Cl)Cl>[CH3:9][O:8][C:6]1[CH:7]=[C:2]([CH3:1])[C:3]([S:11]([N:16]([CH2:17][C:18]2[NH:22][C:21]3[C:23]([C:27]([O:29][CH3:30])=[O:28])=[CH:24][CH:25]=[CH:26][C:20]=3[N:19]=2)[CH3:15])(=[O:13])=[O:12])=[C:4]([CH3:10])[CH:5]=1参加物
4
実験手順
A solution of 2,6-dimethyl-4-methoxybenzenesulfonyl chloride (12.54 mmol, 1.0 eq.) in methylene chloride (12 ml) was added to a cooled solution (0° C.) of methyl 2-((methylamino)methyl)-1H-benzo[d]imidazole-7-carboxylate (12.54 mmol, 1.0 eq.) and TEA (2.5 eq.) in abs. methylene chloride (60 ml). The reaction mixture was stirred at room temperature for 16 h. The reaction mixture was then diluted with methylene chloride and washed successively with water and sat. NaCl solution. The organic phase was dried over Na2SO4 and the solvent was evaporated off in vacuo to obtain the crude product, which led to the desired product by purification by column chromatography (silica gel). Yield: 46%