反应详情

0.2 g (8.4 mmol) of lithium hydroxide was added to a stirred solution of 2,6-bis(4-cyano phenoxy)-nicotinic acid ethyl ester, 1.6 g (4.15 mmol), in a mixture of 5 ml of water and 2.5 ml of THF (2:1) at 5° C. and the contents were stirred for 3 h at RT. The reaction mixture was washed with diethylether. 6 N HCl was added to aqueous layer with stirring until the solution attained a pH of 2. The white precipitate obtained was collected, washed with water and dried under reduced pressure to afford 1.1 g of the required product. Percentage purity (LCMS): 83.2%, (M+1)=357.0+1. 1H NMR (DMSO-d6): δ 6.98 (1H, d), 7.26 (4H, d), 7.80 (4H, d), 13.22 (1H, brs).

1. washThe reaction mixture was washed with diethylether
2. addition6 N HCl was added to aqueous layer
3. stirringwith stirring until the solution
4. customThe white precipitate obtained
5. customwas collected
6. washwashed with water
7. customdried under reduced pressure