反应详情

5-Bromo-2-hydroxy-benzoic acid ethyl ester (40 g, 214 mmol) is suspended in sulfuric acid (200 mL) and the reaction cooled to zero in an ice bath. The reaction is equipped with an overhead stirrer and then the nitric acid (20 mL) in sulfuric acid (40 mL) is added dropwise to the solution over the course of 30 minutes. After the addition the ice bath is removed and the reaction warmed to room temperature. The reaction is stirred at room temperature for 16 hours. When complete the reaction is poured onto crushed ice and the resulting yellow solid is collected by vacuum filtration and washed with ice cold water. The solid dried in vacuum over overnight to give the 45 g (91%) of title compound that is used without further purification. LCMS (ESMS): m/z 291.1 (M+H+).

1. temperaturethe reaction cooled to zero in an ice bath
2. customThe reaction is equipped with an overhead stirrer
3. customis removed
4. additionWhen complete the reaction is poured
5. customonto crushed ice
6. filtrationthe resulting yellow solid is collected by vacuum filtration
7. washwashed with ice cold water
8. customThe solid dried in vacuum over overnight