反应详情

A solution of 1-[2-[(1-naphthalen-1-ylmethyl-piperidin-4-ylmethyl)-(2-trimethylsilanyl-ethoxymethyl)-amino]-1-(2-trimethylsilanyl-ethoxymethyl)-1H-benzimidazol-5-yl]-propan-1-ol (72 mg, 0.10 mmol) in dimethylsulfoxide (1 ml) was added to a solution of 1-hydroxy-1-oxo-1H-1λ5-benzo[d][1,2]iodoxol-3-one (44 mg, 0.157 mmol) in dimethylsulfoxide (1 ml), and the mixture was stirred at room temperature for 18 hours. The reaction mixture was poured into ice water (50 ml) and stirred at room temperature for 30 minutes, after which ethyl acetate was added and stirring was continued vigorously for 10 minutes for extraction. After washing with saturated aqueous sodium bicarbonate and then with saturated brine, the mixture was dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure to obtain 1-[2-[(1-naphthalen-1-ylmethyl-piperidin-4-ylmethyl)-(2-trimethylsilanyl-ethoxymethyl)-amino]-1-(2-trimethylsilanyl-ethoxymethyl)-1H-benzimidazol-5-yl]-propan-1-one.

1. stirringstirred at room temperature for 30 minutes
2. stirringstirring
3. extractionwas continued vigorously for 10 minutes for extraction
4. washAfter washing with saturated aqueous sodium bicarbonate
5. dry with materialwith saturated brine, the mixture was dried over anhydrous sodium sulfate
6. distillationthe solvent was distilled off under reduced pressure