反应详情

4.8 g of iron powder and 0.45 ml of concentrated hydrochloric acid were added to a mixture solvent of 50 ml of water and 10 ml of ethanol, and the solution was heated at 80°-90° C. 6.69 g (31 mmol) of 4-chloro-3-fluoro-2-(2-hydroxyethyl)nitrobenzene was added to the solution through 10 minutes, and the solution was heated for 1 hour as was. After air-cooling, 100 ml of ethyl acetate was added to the solution, and insoluble matter was filtered. The organic layer was separated and was washed with aqueous 10% sodium hydrogen carbonate solution. After drying over magnesium sulfate, the solvent was removed by distillation to obtain 4.68 g of the subject compound (126) in a 80% yield.

1. temperaturethe solution was heated at 80°-90° C
2. temperaturethe solution was heated for 1 hour
3. temperatureAfter air-cooling
4. filtrationwas filtered
5. customThe organic layer was separated
6. washwas washed with aqueous 10% sodium hydrogen carbonate solution
7. dry with materialAfter drying over magnesium sulfate
8. customthe solvent was removed by distillation