反应详情

A mixture of 1-chloro-2-isothiocyanatobenzene 1 (3 g, 17.68 mmol) and isonicotinohydrazide 2 (2.43 g, 17.68 mmol) in acetonitrile was stirred at ambient temperature for 18 hours, concentrated to dryness, and 100 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 4 (4.3 g). Yield: 86%.

1. concentrationconcentrated to dryness, and 100 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