反应详情

To a suspension of trans-3-acetoxy-4-(2-cyanoiminoimidazolidin-1-yl)-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran-6-carbonitrile (0.35 g) in toluene (7 ml) was added 1,8-diazabicyclo[5.4.0]undec-7-ene (0.19 ml) and the mixture was stirred under reflux for 2.5 hours. The solvent was evaporated in vacuo and the residue was dissolved in a mixture of ethyl acetate and water. The organic layer was separated, washed with brine, dried over anhydrous magnesium sulfate, and evaporated in vacuo. The residue was recrystallized from ethanol to give 4-(2-cyanoiminoimidazolidin-1-yl)-2,2-dimethyl-2H-1-benzopyran-6-carbonitrile (0.17 g).

1. temperatureunder reflux for 2.5 hours
2. customThe solvent was evaporated in vacuo
3. dissolutionthe residue was dissolved in a mixture of ethyl acetate and water
4. customThe organic layer was separated
5. washwashed with brine
6. dry with materialdried over anhydrous magnesium sulfate
7. customevaporated in vacuo
8. customThe residue was recrystallized from ethanol