反应详情

A mixture of 1-chloro-2-isothiocyanatobenzene 1 (0.4 g, 2.33 mmol) and 2-chloropyridine-4-carbohydrazide 11 (0.4 g, 2.33 mmol) in DMF was stirred at ambient temperature for 18 hours, concentrated to dryness, and 20 mL of 10% K2CO3 (aq.) was added. The resulting mixture was stirred under reflux for 6 hours. The clear solution was cooled to ambient temperature, washed with ether, and acidified with 1N HCl. The solid was collected, washed with H2O and ether, and dried to afford compound 13 (4.3 g). Yield: 86%.

1. concentrationconcentrated to dryness, and 20 mL of 10% K2CO3 (aq.)
2. additionwas added
3. stirringThe resulting mixture was stirred
4. temperatureunder reflux for 6 hours
5. temperatureThe clear solution was cooled to ambient temperature
6. washwashed with ether
7. customThe solid was collected
8. washwashed with H2O and ether
9. customdried