反应详情

Et3N (10 ml) was added to a solution of ethyl 2-cyanonicotinate (1.9 g, 10.78 mmol) in 20 ml of pyridine. Hydrogen sulfide was passed through the reaction mixture at 5° C. for 20 minutes, then the mixture was stirred for 1 hour at room temperature. For work up the solution was purged with nitrogen for 30 minutes, evaporated to dryness, and the remaining solid dissolved in 200 ml of dichloromethane. The organic layer was washed successively with water and brine, dried, evaporated and treated with ethylacetate to give 2.15 g of a red oil which was reacted without further purification.

1. customFor work up the solution was purged with nitrogen for 30 minutes
2. customevaporated to dryness
3. dissolutionthe remaining solid dissolved in 200 ml of dichloromethane
4. washThe organic layer was washed successively with water and brine
5. customdried
6. customevaporated
7. additiontreated with ethylacetate