反应详情

36.00 g (0.166 mol) of N-(4-nitro-phenyl)-methanesulphonic acid amide was dissolved in 2000 mL acetone. The solution was combined with 47.8 g (0.332 mol) of 1-chloro-2-dimethylaminoethane * HCl, 68.8 g (0.498 mol) of potassium carbonate, 5.0 g (0.033 mol) of sodium iodide and 50 mL water. It was refluxed for 16 hours with stirring. After the addition of another 23.9 g (0.166 mol) of 1-chloro-2-dimethylaminoethane * HCl, 45.9 g (0.332 mol) of potassium carbonate and 5.0 g (0.033 mol) of sodiumiodide, the mixture was refluxed for 5 hours with stirring. At RT the inorganic salts were filtered off. The filtrate was evaporated down i. vac. and the residue dissolved in EtOAc. The org. phase was washed 2× with semisat. aqueous sodium chloride solution, dried over magnesium sulphate, filtered and evaporated down i. vac.

1. temperatureIt was refluxed for 16 hours
2. temperaturethe mixture was refluxed for 5 hours
3. stirringwith stirring
4. filtrationAt RT the inorganic salts were filtered off
5. customThe filtrate was evaporated down i
6. dissolutionand the residue dissolved in EtOAc
7. washphase was washed 2× with semisat
8. dry with materialaqueous sodium chloride solution, dried over magnesium sulphate
9. filtrationfiltered
10. customevaporated down i