反应详情

温度

50 °C

Dissolved 5.00 g (23.7 mmol) methyl 4-ethoxy-3-methoxybenzoate in 25 ml acetic acid under N2 and added 6.1 ml (95.1 mmol) 69% nitric acid dropwise over 30 minutes. Heated to 50° C. for 1.5 hours and poured onto ice bath. Extracted with chloroform, washed with dilute sodium hydroxide solution and filtered through magnesium sulfate. Stripped solvent and dried in vacuo, giving 5.268 of off-white solid: mass spectrum (electrospray m/e): M+H=255.8.

1. additionpoured onto ice bath
2. extractionExtracted with chloroform
3. washwashed with dilute sodium hydroxide solution
4. filtrationfiltered through magnesium sulfate
5. customdried in vacuo
6. customgiving 5.268 of off-white solid