反应详情

To a solution of 51.0 g (245.1 mmol) of 6-bromo-isoquinoline (3) in 800 ml of dichloromethane were added under mechanical stirring 90.6 g (367.6 mmol) of 3-chloro-benzenecarboperoxoic acid (70%). After stirring for 4 h at room temperature and standing overnight, saturated sodium hydrogen carbonate-solution was added until two clear layers were obtained. The dichloromethane solution was separated and washed with saturated NaCl-solution. The aqueous layers were extracted with a chloroform/isopropanol (3:1) mixture and the organic layers were combined, washed again with saturated NaCl-solution, dried over magnesium sulfate and evaporated. The obtained crude product (53.0 g) was used without further purification. Rt=0.89 min (Method C). Detected mass: 226.2 (M+H+).

1. waitstanding overnight
2. customwere obtained
3. customThe dichloromethane solution was separated
4. washwashed with saturated NaCl-solution
5. extractionThe aqueous layers were extracted with a chloroform/isopropanol (3:1) mixture
6. washwashed again with saturated NaCl-solution
7. dry with materialdried over magnesium sulfate
8. customevaporated