反应详情

温度

100 °C

A mixture of 3,4-epoxy-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran-6-carbonitrile (0.51 g), 2-cyanoiminothiazolidine (0.64 g) and pyridine (4.1 ml) was heated at 100° C. for 1.5 hours. Pyridine was removed under reduced pressure. The residue was diluted with ethyl acetate (20 ml). The solution was washed with water (20 ml and 15 ml), 5% aqueous hydrochloric acid (15 ml×2) and saturated aqueous sodium chloride (15 ml) successively, treated with charcoal, and then dried over anhydrous magnesium sulfate. The solvent was evaporated in vacuo, and the residue was triturated with ethyl acetate, to give trans-4-(2-cyanoiminothiazolidin-3-yl)-3,4-dihydro-3-hydroxy-2,2-dimethyl-2H-1-benzopyran-6-carbonitrile (0.47 g).

1. customPyridine was removed under reduced pressure
2. additionThe residue was diluted with ethyl acetate (20 ml)
3. washThe solution was washed with water (20 ml and 15 ml), 5% aqueous hydrochloric acid (15 ml×2) and saturated aqueous sodium chloride (15 ml) successively
4. additiontreated with charcoal
5. dry with materialdried over anhydrous magnesium sulfate
6. customThe solvent was evaporated in vacuo
7. customthe residue was triturated with ethyl acetate