反应详情

Phosphorus pentachloride (22 g) was added to 19.3 g of p-nitrocinnamic acid suspended in 300 ml of ethyl acetate, and the resulting mixture was stirred at room temperature for 1 hour. After the reaction, the solvent was distilled off under reduced pressure, upon which p-nitrocinnamoyl chloride precipitated. The precipitates thus obtained were dissolved in 300 ml of ethyl acetate, and 9.4 g of phenol was added to the resulting solution, after which 12 g of triethylamine was slowly added thereto at room temperature with stirring. After reaction at room temperature for 1 hour, the reaction mixture was washed with 10% HCl, 10% NaOH and water in this order and dried on anhydrous magnesium sulfate. The solvent was then distilled off under reduced pressure, to obtain phenyl p-nitrocinnamate. Yield: 25.5 g (95%); melting point: 151°-152° C.; IR (cm-1): 1720, 1529, 1345.

1. customAfter the reaction
2. distillationthe solvent was distilled off under reduced pressure, upon which p-nitrocinnamoyl chloride
3. customprecipitated
4. customThe precipitates thus
5. customobtained
6. stirringat room temperature with stirring
7. customAfter reaction at room temperature for 1 hour
8. washthe reaction mixture was washed with 10% HCl, 10% NaOH and water in this order
9. dry with materialdried on anhydrous magnesium sulfate
10. distillationThe solvent was then distilled off under reduced pressure