反应详情

Dissolve 2-bromo-1-(5-chloro-2-methoxy-phenyl)-ethanone (17.07 g, 64.78 mmol) in 150 mL of CHCl3 and add hexamethylenetetramine (9.09 g, 64.84 mmol) to the reaction mixture. Allow the reaction to stir at ambient temperature for 23 hours. Collect the solids via filtration and wash the solids with Et2O. Slurry the solid in 100 mL of MeOH and add 50 mL of concentrated HCl to it dropwise. Heat the reaction to reflux and allow it to stir for 23 hours. Cool the reaction to ambient temperature and filter off the solids. Slurry the filtrate in MeOH and again collect the solids via filtration. Concentrate the filtrate to afford 10.99 g of 2-amino-1-(5-chloro-2-methoxy-phenyl)-ethanone hydrochloride.

1. customthe reaction
2. customCollect the solids
3. filtrationvia filtration
4. washwash the solids with Et2O
5. additionadd 50 mL of concentrated HCl to it dropwise
6. temperatureHeat
7. customthe reaction
8. temperatureto reflux
9. stirringto stir for 23 hours
10. temperatureCool
11. customthe reaction to ambient temperature
12. filtrationfilter off the solids
13. customSlurry the filtrate in MeOH and again collect the solids
14. filtrationvia filtration
15. concentrationConcentrate the filtrate