反应详情

To a solution 4-cyanophenol (CAS Reg. No. 767-00-0, 1.2 g), 2-chloro-4-fluoroacetophenone (CAS Reg. No. 700-35-6, 1.7 g) in DMA (10 ml) was added K2CO3 (1.66 g). The mixture is refluxed for 5 h. TLC (heptane/EtOAc 2:1) showed complete conversion. Water was added and the mixture was extracted with DCM. The combined organic layers were dried over Na2SO4 and then concentrated to an oil. The residue was purified by flash chromatography (SiO2, EtOAc/heptane 1:2) to give the title compound (1.8 g) as yellow oil. MS (m/e)=272.2 [M+H+].

1. temperatureThe mixture is refluxed for 5 h
2. extractionthe mixture was extracted with DCM
3. dry with materialThe combined organic layers were dried over Na2SO4
4. concentrationconcentrated to an oil
5. customThe residue was purified by flash chromatography (SiO2, EtOAc/heptane 1:2)