反应详情

To a stirring solution of tert-butyl (2S,4S)-2-(5-iodo-1H-benzimidazol-2-yl)-4-methyl-pyrrolidine-1-carboxylate (3.70 g, 8.659 mmol) in dichloromethane (34 mL) is added TFA (17.22 mL, 223.5 mmol) and stirred at rt for 1 h. The reaction mixture is concentrated, azeotroped 2× with toluene and dried in vacuo. The residue is diluted with dichloromethane (200 mL), washed 2× with saturated sodium bicarbonate and brine and then dried over sodium sulfate. The organic is evaporated to give 5-iodo-2-[(2S,4S)-4-methylpyrrolidin-2-yl]-1H-benzimidazole (2.32 g, 82%).

1. concentrationThe reaction mixture is concentrated
2. customazeotroped 2× with toluene
3. customdried in vacuo
4. additionThe residue is diluted with dichloromethane (200 mL)
5. washwashed 2× with saturated sodium bicarbonate and brine
6. dry with materialdried over sodium sulfate
7. customThe organic is evaporated