反应详情

Potassium carbonate 1.58 g (11.5 mmol) was added to a stirred solution of 2,6-dichloro-nicotinic acid ethyl ester 1.0 g (4.6 mmol) in 5 ml of DMF and stirred for 10 min. 4-Hydroxy-benzonitrile 1.36 g (11.5 mmol), dissolved in 5 ml of DMF, was added dropwise to the stirred DMF solution and the flask was stirred at 80° C. for 4 h. The reaction mixture was poured into ice-cold water and the result was partitioned using ethyl acetate. The organic phase was washed with 1 M of Na2CO3 and saturated brine solution, dried over sodium sulphate and concentrated. The oily residue was purified by column chromatography using hexane-ethyl acetate (10:2) to afford 1.6 g of the required product. Percentage purity: 84.8%, (M+1)=385.1. 1H NMR (DMSO-d6): 1.36 (3H, t), 4.22 (214, q), 6.78 (1H, d), 7.06 (4H, d), 7.58 (4H, d), 8.21 (1H, d).

1. stirringthe flask was stirred at 80° C. for 4 h
2. additionThe reaction mixture was poured into ice-cold water
3. customthe result was partitioned
4. washThe organic phase was washed with 1 M of Na2CO3 and saturated brine solution
5. dry with materialdried over sodium sulphate
6. concentrationconcentrated
7. customThe oily residue was purified by column chromatography