反应详情

温度

135 °C

To a solution of 685 mg (2.531 mmol) 6-chloro-4-cyclopropyl-7-fluoro-1-hydroxy-1,4-dihydro-quinoxaline-2,3-dione in 10 mL N,N-dimethylformamide was added 996 mg (3.796 mmol) triphenylphosphine. The reaction mixture was stirred for 4 hours at 135° C. The reaction mixture was concentrated under vacuum (15 mbar/55° C.). The residue was suspended in 20 mL dichloromethane. The suspension was stirred for 30 min at 0° C. and filtered and washed with 20 mL dichloromethane. White solid (63%). MS (ESI): m/z=255.034 [M+H]+.

1. concentrationThe reaction mixture was concentrated under vacuum (15 mbar/55° C.)
2. stirringThe suspension was stirred for 30 min at 0° C.
3. filtrationfiltered
4. washwashed with 20 mL dichloromethane