反应详情

温度

50 °C

To a solution of (R)-tert-butyl 3-(1-(2-(dimethylamino)ethyl)-2-neopentyl-1H-benzo[d]imidazol-5-ylsulfonyl)pyrrolidine-1-carboxylate (STEP B, 612 mg, 1.24 mmol) in methanol (5 mL) was added chlorotrimethylsilane (749 microL, 6.21 mmol). The mixture was stirred at 50° C. for 3 h. The mixture was concentrated in vacuo. To the residue was added 2 mol/L sodium hydroxide aqueous solution to pH>7 and the mixture was extracted with ethyl acetate (150 mL). The organic layer was washed with brine and dried over sodium sulfate. The resulting solution was concentrated to give the title compound (453 mg, 93%) as an oil.

1. concentrationThe mixture was concentrated in vacuo
2. additionTo the residue was added 2 mol/L sodium hydroxide aqueous solution to pH>7
3. extractionthe mixture was extracted with ethyl acetate (150 mL)
4. washThe organic layer was washed with brine
5. dry with materialdried over sodium sulfate
6. concentrationThe resulting solution was concentrated