反应详情

To a solution of 1.8 g. of 2-phenylethenesulfonamide and 4.8 g. of 1,1-diphenyl-3-(bicyclo[2.2.1]hept-2-en-5-ylmethyl)urea in 20 ml. of N,N-dimethylformamide, is added, with stirring 0.64 g. of a 56.6% dispersion of sodium hydride in mineral oil. The mixture is stirred at ambient temperature overnight, during which time a heavy precipitate forms. To the reaction mixture is then added 200 ml. of ether. After stirring for 15 minutes, the precipitate is filtered off. It is dissolved in 50 ml. of water, and then the crude product is precipitated by acidification usng concentrated hydrochloric acid. It is filtered off and recrystallized from aqueous acetone. The yield is 1.9 g. (56%) of a solid, m.p. 161°-163.5° C.

1. stirringThe mixture is stirred at ambient temperature overnight, during which time a heavy precipitate forms
2. additionTo the reaction mixture is then added 200 ml
3. stirringAfter stirring for 15 minutes
4. filtrationthe precipitate is filtered off
5. dissolutionIt is dissolved in 50 ml
6. customof water, and then the crude product is precipitated by acidification usng concentrated hydrochloric acid
7. filtrationIt is filtered off
8. customrecrystallized from aqueous acetone