反应详情

11.1 g (41.07 mmol) of 5-fluoro-1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridine-3-carbonitrile (Example 8A) were added to 2.22 g (41.07 mmol) of sodium methoxide in methanol (270 ml), and the mixture was stirred at RT for 2 h. 2.64 g (49.29 mmol) of ammonium chloride and acetic acid (9.17 ml) were then added, and the mixture was heated to reflux overnight. It was then concentrated to dryness and the residue was taken up in water (100 ml) and ethyl acetate (100 ml) and adjusted to a pH of 10 using 2N aqueous sodium hydroxide solution. The mixture was stirred vigorously at RT for about 1 h. The resulting suspension was filtered with suction and washed through with ethyl acetate (100 ml), with water (100 ml) and once more with ethyl acetate (100 ml). The residue was dried under high vacuum over phosphorus pentoxide.

1. temperaturethe mixture was heated
2. temperatureto reflux overnight
3. concentrationIt was then concentrated to dryness
4. stirringThe mixture was stirred vigorously at RT for about 1 h
5. filtrationThe resulting suspension was filtered with suction
6. washwashed through with ethyl acetate (100 ml), with water (100 ml) and once more with ethyl acetate (100 ml)
7. dry with materialThe residue was dried under high vacuum over phosphorus pentoxide