反应详情

To a stirred solution of 2,2,2-trichloro-1-(4-iodo-1H-pyrrol-2-yl)ethanone (68 g, 201 mmol, 1.0 equivalent) in dry methanol (400 mL) under nitrogen, was added a solution of sodium methoxide in methanol (4.37 M, 54 mL, 235 mmol, 1.2 equivalents) over 10 minutes. The resulting mixture was stirred at room temperature for 1 hour. The volatiles were removed under reduced pressure and the crude was then partitioned between water and tert-butylmethyl ether. The organic phase was separated, washed two times with water, saturated sodium chloride, dried over sodium sulfate, filtered and concentrated under vacuum to afford the title compound (48 g, 96%) as a colorless solid, that was used directly without further purification.

1. customThe volatiles were removed under reduced pressure
2. customthe crude was then partitioned between water and tert-butylmethyl ether
3. customThe organic phase was separated
4. washwashed two times with water, saturated sodium chloride
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated under vacuum