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 added, and the mixture was heated at reflux overnight. The mixture was then concentrated to dryness, and the residue was taken up in water (100 ml) and ethyl acetate (100 ml) and adjusted to pH 10 with 2 N aqueous sodium hydroxide solution. The mixture was stirred at RT for about 1 h. The resulting suspension was filtered off with suction and washed with ethyl acetate (100 ml), water (100 ml) and once more with ethyl acetate (100 ml). The residue was dried over phosphorus pentoxide under high vacuum.

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