136592-00-2

5326-23-8

79-37-8

136592-00-2

The general procedure for the synthesis of 2-chloro-1-(6-chloropyridin-3-yl)ethanone from 6-chloronicotinic acid and oxalyl chloride is as follows: 1. 6-Chloronicotinic acid (1.58 g, 10.0 mmol) was suspended in dichloromethane (50 mL) and DMF (4 drops) was added as catalyst. 2. oxalyl chloride (1.53 g, 12.0 mmol) was slowly added to the suspension with stirring. 3. After stirring the reaction mixture for 2.5 hours, trimethylsilyl diazomethane (25 mL, 2.0 M solution, 50.1 mmol) was added. 4. The reaction was continued for 2 hr and then HCl gas was passed for 10 min. 5. After completion of the reaction, the reaction mixture was washed sequentially with saturated sodium bicarbonate solution and saturated sodium chloride solution. 6. The organic phase was dried with magnesium sulfate, filtered and concentrated to give 2-chloro-1-(6-chloropyridin-3-yl)ethanone (1.85 g, 97% yield) as a light brown solid. Product characterization: ESI-LRMS m/e calculated value C7H5Cl2NO [M+] 190, measured value 191 [M+H+].