반응 #727907

반응 방정식

4-(3-fluorophenyl)-6-methoxy-2-oxo-1,2-dihydroquinoline-3-carbonitrile

phosphorus oxytrichloride

→

titled compound

수율 66.0%

2-Chloro-4-(3-fluorophenyl)-6-methoxyquinoline-3-carbonitrile

수율 66.0%

용매

EtOAc

반응 조건

후처리

1. 1
   온도cooled to 0° C.
2. 2
   기타quenched by the careful addition of saturated NaHCO3 solution
3. 3
   세척The organic phase was washed with brine
4. 4
   건조dried over Na2SO4
5. 5
   여과filtered
6. 6
   농축concentrated in vacuo

실험 절차

A solution of 4-(3-fluorophenyl)-6-methoxy-2-oxo-1,2-dihydroquinoline-3-carbonitrile (1.10 g, 3.74 mmol) in 30 mL of phosphorus oxytrichloride was heated in a sealed pressure tube at 90° C. for 2 hours. The solution was cooled to room temperature and allowed to stand overnight. The mixture was diluted with EtOAc, cooled to 0° C., and quenched by the careful addition of saturated NaHCO3 solution. The organic phase was washed with brine, dried over Na2SO4, filtered, and concentrated in vacuo to provide the titled compound (774 mg, 66%) ESI+ MS: 313.0 [M+H]+.

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