反应详情

2.6 g (17.5 mmol) 2-mercaptopyridine-1-oxid was dissolved in 30.0 ml bromotrichloromethane and heated to reflux. A mixture of 4.04 g (15 mmol) 3,5-diacetoxybenzoylchloride and 433 mg (2.5 mmol) 2,2′-azobisisobutyronitril dissolved in 30.0 ml bromotrichlioromethane were added dropwise at the same temperature. After additional 2 hours of refluxing the reaction mixture was cooled to room temperature and concentrated in vacuum. Chromatographic purification over silica gel employing a 9:1 (v/v) mixture of n-hexane and ethyl acetate as eluting agent yielded 2.4 g of 3,5-diacetoxybromobenzene (8.7 mmol, 58%).

1. temperatureheated to reflux
2. dissolutiondissolved in 30.0 ml bromotrichlioromethane
3. additionwere added dropwise at the same temperature
4. temperatureAfter additional 2 hours of refluxing the reaction mixture
5. concentrationconcentrated in vacuum
6. customChromatographic purification over silica gel employing
7. additiona 9:1 (v/v) mixture of n-hexane and ethyl acetate
8. washas eluting agent