反应详情

温度

0 °C

2.1 g of this ethyl 3-amino-3-(2-fluorophenyl)-2-propenoate was added dropwise to a solution of 0.5 g of sodium hydride (purity: 55%) in 20 ml of dimethylformamide with stirring at 0° C. The resulting solution was further stirred at room temperature for 15 minutes and then cooled to -30° C. and added dropwise with 20 ml of a toluene solution of 1.7 g of 2-fluoro-4-chlorophenyl isocyanate. The resultant solution was heated to room temperature and stirred at 80° C. for 30 minutes. Then the solvent was distilled away under reduced pressure and 100 ml of water was added to the residue to dissolve it. This aqueous solution was washed twice with diethyl ether and added to a mixed solution of 50 g of ice and 20 ml of concentrated hydrochloric acid. The precipitated crystals were filtered out and dried under the reduced pressure to obtain 3.0 g of a crude product. This crude product was washed with heated diisopropyl ether and then dried to obtain 2.4 g of the objective compound.

1. stirringThe resulting solution was further stirred at room temperature for 15 minutes
2. temperaturecooled to -30° C.
3. stirringstirred at 80° C. for 30 minutes
4. distillationThen the solvent was distilled away under reduced pressure and 100 ml of water
5. additionwas added to the residue
6. dissolutionto dissolve it
7. washThis aqueous solution was washed twice with diethyl ether
8. additionadded to a mixed solution of 50 g of ice and 20 ml of concentrated hydrochloric acid
9. filtrationThe precipitated crystals were filtered out
10. customdried under the reduced pressure
11. customto obtain 3.0 g of a crude product
12. washThis crude product was washed with heated diisopropyl ether
13. customdried