反应详情

温度

160 °C

The above 5-bromo-2-chlorophenylacetonitrile was added to water (90 ml)-sulfuric acid (75 ml), and the mixture was stirred under heating at 160° C. overnight. The mixture was further diluted with water, and cooled to 0° C. The solvent was removed by decant, and the residue was dissolved in diethyl ether. The solution was washed with water and brine, and extracted with 10% sodium hydroxide. To the extract was added concentrated hydrochloric acid to make the solution acidic. The precipitates were collected by filtration, and purified by silica gel column chromatography (chloroform) to give 5-bromo-2-chlorophenylacetic acid (6.67 g) as colorless crystals. ESI-Mass m/Z 247/249 (M−H).

1. temperaturecooled to 0° C
2. customThe solvent was removed
3. customby decant
4. dissolutionthe residue was dissolved in diethyl ether
5. washThe solution was washed with water and brine
6. extractionextracted with 10% sodium hydroxide
7. additionTo the extract was added concentrated hydrochloric acid
8. filtrationThe precipitates were collected by filtration
9. custompurified by silica gel column chromatography (chloroform)