反应详情

温度

100 °C

To a suspension of trans-3-acetoxy-4-(2-cyanoimino-3-methylimidazolidin-1-yl)-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran-6-carbonitrile (0.45 g) in toluene (9 ml) was added 1,8-diazabicyclo[5.4.0]undec-7-ene (0.23 ml), and the reaction mixture was stirred at 100° C. for 2 hours and 40 minutes. The solvent was removed under reduced pressure. The residue was poured into water (30 ml) and then extracted with ethyl acetate (45 ml). The organic layer was washed with brine (30 ml), dried over magnesium sulfate and evaporated in vacuo. The residue was recrystallized from ethanol to give 4-(2-cyanoimino-3-methylimidazolidin-1-yl)-2,2-dimethyl-2H-1-benzopyran-6-carbonitrile (0.27 g).

1. customThe solvent was removed under reduced pressure
2. additionThe residue was poured into water (30 ml)
3. extractionextracted with ethyl acetate (45 ml)
4. washThe organic layer was washed with brine (30 ml)
5. dry with materialdried over magnesium sulfate
6. customevaporated in vacuo
7. customThe residue was recrystallized from ethanol