反应详情

温度

95 °C

To a mixture of 3-chloro-4-hydroxy-5-methoxybenzoic acid (2.468 mmol, 500 g), thiosemicarbazide (5b) (2.468 mmol, 427 mg) in dioxane (10 mL) at 65° C., POCl3 (3.2 mmol, 300 μL) was added, and the mixture was warmed at 95° C. for 3 hours 30 minutes. The solvent was removed by distillation under reduced pressure to give a crude material which was basified with a solution of diluted NH4OH. The precipitate obtained was collected by filtration, washed with water before drying under vacuum over P2O5 to give 675 mg of the desired product. Yield: 80%.

1. customThe solvent was removed by distillation under reduced pressure
2. customto give a crude material which
3. customThe precipitate obtained
4. filtrationwas collected by filtration
5. washwashed with water
6. dry with materialbefore drying under vacuum over P2O5