反应详情

1.16 g (10.8 mmol) 1,2-phenylene diamine was dissolved in 10 ml dimethyl formamide, 2.1 g (15 mmol) potassium carbonate and 1.47 ml (10.8 mmol) 1-bromo-1-phenylethane were added with stirring. After 8 hours (h) at rt, most of the starting materials were consumed. Potassium bromide was filtered off, the solvent removed, the mixture redissolved in 20 ml THF and then 1,15 g (8 mmol) 4-cyanophenylisocyanate were slowly added and stirred for another 50 h at rt. The mixture was worked up by filtration, evaporated to dryness, dissolved in ethyl acetate and washed with diluted HCl, sodium carbonate solution and brine.

1. custommost of the starting materials were consumed
2. filtrationPotassium bromide was filtered off
3. customthe solvent removed
4. dissolutionthe mixture redissolved in 20 ml THF
5. stirringstirred for another 50 h at rt
6. filtrationThe mixture was worked up by filtration
7. customevaporated to dryness
8. dissolutiondissolved in ethyl acetate
9. washwashed with diluted HCl, sodium carbonate solution and brine