反应详情

温度

140 °C

In a stirred suspension of 96.37 g potassium carbonate in 700 gm dimethyl formamide, 100 gm 2-chloro nicotinic acid was charged. A solution of 82.38 g benzyl mercaptan in 300 gm dimethyl formamide was added in a period of two hours maintaining reaction temperature 80-90° C. The temperature of the reaction was raised up to 140° C. and then maintained for another three hours. 500 g water was added after completion of the reaction and solvent recovery. Product precipitation achieved by lowering the pH of the reaction mass by using dilute HCl. Product 2-(Phenyl methyl thio)-3-pyridine carboxylic acid precipitated completely till pH 4.5. After filtration and washing, cake was dried to get 110 g white to off white solid product 2-(Phenyl methyl thio)-3-pyridine carboxylic acid with 71.49% yield (Assay by HPLC 99.23%).

1. additionwas charged
2. temperaturemaintaining
3. customreaction temperature 80-90° C
4. temperaturemaintained for another three hours
5. customafter completion of the reaction and solvent recovery
6. customProduct precipitation
7. customProduct 2-(Phenyl methyl thio)-3-pyridine carboxylic acid precipitated completely till pH 4.5
8. filtrationAfter filtration
9. washwashing
10. customcake was dried