反应详情

ba) A suspension of 580.1 mg of 2-bromo-4'-hydroxy-3'-methoxy-5'-nitroacetophenone in 10 ml of ethanol is treated with 443.8 mg of selenium dioxide and heated under reflux for 71 hours. Thereafter, the selenium is removed by filtration and the filtrate is evaporated. The residue is dissolved in methylene chloride, washed with saturated sodium chloride solution, dried over sodium sulfate, filtered and evaporated. There is obtained ethyl 4-hydroxy-3-methoxy-5-nitrophenylglyoxylate of m.p. 165°-167° (from ethanol).

1. temperatureheated
2. temperatureunder reflux for 71 hours
3. customThereafter, the selenium is removed by filtration
4. customthe filtrate is evaporated
5. dissolutionThe residue is dissolved in methylene chloride
6. washwashed with saturated sodium chloride solution
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. customevaporated