反应详情

温度

80 °C

To 1,3-dimethylthiourea (2.489 g, 23.89 mmol) and triethylamine (2.78 ml, 19.91 mmol) in dry toluene was added 2,2,7-trifluoro-6-isocyanato-4-(prop-2-ynyl)-2H-benzo[b][1,4]oxazin-3(4H)-one (5.62 g, 19.91 mmol) in dry toluene. Hereto was subsequently added carbonyldiimidazole (CDI; 6.46 g, 39.8 mmol) and the resulting mixture was stirred at 80° C. overnight. Then the reaction mixture was cooled to room temperature and poured into ethyl acetate/water under stirring. The layers were separated and the aqueous layer was extracted with dichloromethane. The combined extracts were washed with brine, dried with Na2SO4 and concentrated to yield 14.4 g.

1. temperatureThen the reaction mixture was cooled to room temperature
2. stirringunder stirring
3. customThe layers were separated
4. extractionthe aqueous layer was extracted with dichloromethane
5. washThe combined extracts were washed with brine
6. dry with materialdried with Na2SO4
7. concentrationconcentrated
8. customto yield 14.4 g