反应详情

To trans-4-amino-6-cyano-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran-3-ol (1.09 g) and triethylamine (0.77 ml) in dichloromethane (20 ml), cooled in an ice bath, was added ethylchloroformate (0.67 ml). The mixture was allowed to attain room temperature and stirred for 2 days. The reaction mixture was washed with water and dried over anhydrous magnesium sulphate. Filtration and evaporation and chromatography (chromatotron, gradient elution: 10-30% Ethyl acetate-pentate) gave one fraction (456 mg) which was recrystallised from ethyl acetate-pentane to give the compound of this example (319 mg); mp 147°-148° C.

1. customto attain room temperature
2. washThe reaction mixture was washed with water
3. dry with materialdried over anhydrous magnesium sulphate
4. filtrationFiltration and evaporation and chromatography (chromatotron, gradient elution: 10-30% Ethyl acetate-pentate)
5. customgave one fraction (456 mg) which
6. customwas recrystallised from ethyl acetate-pentane
7. customto give the compound of this example (319 mg)