反应详情

A solution of 5-Bromo-4-(2,2,2-trifluoro-ethoxy)-pyridine-2-carbonitrile (Example 78c, 1 g, 3.56 mmol) in sulfuric acid 97% (5 ml) was stirred at 120° C. for 2 h and a 6.0M aqueous solution of sodium nitrite (2.08 ml, 12.5 mmol, Eq: 3.5) was then slowly added to it at r.t. The resulting reaction mixture was stirred at room temperature for 30 minutes and stirred at 80° C. for 1 hour. The reaction was diluted by addition of 20 gr of ice and the pH was adjusted to 1-2 by addition of sodium hydroxide pellets by portions. A precipitate formed and was filtered off, dried under high vacuum to yield the title compound (1.02 g, 95%) as a white solid. MS (ESI, m/z): 300.2 (M+H+).

1. customThe resulting reaction mixture
2. stirringstirred at 80° C. for 1 hour
3. customA precipitate formed
4. filtrationwas filtered off
5. customdried under high vacuum