反应详情

温度

100 °C

To a mixture of 2-chloro-5-(4-(difluoromethoxy)phenyl)pyrimidine 30 (3.2 mmol) and 3-aminophenol (6.42 mmol) in 1,4-dioxane (5 mL) is added p-TSA (5.4 mmol). The reaction mixture is heated at 100° C. for 12 h. After this time, the reaction is diluted with a 2M solution of Na2CO3 and extracted with DCM (3×50 mL). The organic layer is washed with brine, dried over Na2SO4, and concentrated. Purification by short SiO2 chromatography using a DCM:EtOAc=7:3 as eluant affords (3-(5-(4-(difluoromethoxy)phenyl)pyrimidin-2-ylamino)phenol 39. MS (m/z) (M+1)+: 330.1.

1. extractionextracted with DCM (3×50 mL)
2. washThe organic layer is washed with brine
3. dry with materialdried over Na2SO4
4. concentrationconcentrated
5. customPurification by short SiO2 chromatography