反应详情

温度

95 °C

To a mixture of 3-chloro-2,6-dimethoxybenzoic acid (2.3 mmol, 500 mg), thiosemicarbazide (5b) (2.3 mmol, 399 mg) in anhydrous dioxane (10 mL) at 70° C. to 80° C., POCl3 (2.3 mmol, 215 μL) was added, and the mixture was warmed at 95° C. for 5 hours. The solvent was removed by distillation under reduced pressure to give a crude material which was basified at pH 8-7 with a saturated solution of NaHCO3. The precipitate obtained was collected by filtration, washed with water, and dried under vacuum. The solid was subjected to flash chromatography eluting with ethyl acetate/cyclohexane to give 115 mg of the title compound. Yield: 14%.

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. customdried under vacuum
7. washeluting with ethyl acetate/cyclohexane