反应详情

温度

100 °C

15 g of pyridine-2-carboxylic acid (121.8 mmol) were dissolved in 150 ml of dimethylformamide. At room temperature, 29.6 g (181.8 mmol) of carbonyldiimidazole were slowly added, during which gas was evolved. Reaction was allowed to take place at 100° C. for 30 min, and then 25.6 g (242.7 mmol) of 4-methyl-3-thiosemicarbazide were added, and the mixture was stirred at 100° C. for a further 2 h. The reaction mixture was mixed with 300 ml of water. After cooling in an ice bath, the precipitated crystals were filtered off with suction and washed with a little water. The crystals were taken up in 390 ml of 1M sodium bicarbonate solution and heated to reflux for 3 h.

1. customReaction
2. customat 100° C.
3. customfor 30 min
4. temperatureAfter cooling in an ice bath
5. filtrationthe precipitated crystals were filtered off with suction
6. washwashed with a little water
7. temperatureheated
8. temperatureto reflux for 3 h.