反应详情

500 mg (1.37 mmol)of N-[3-(1,1,2,2-tetrafluoro-ethoxy)-phenyl]-4(4-pyridyl)-2-pyrimidineamine are suspended in 10 ml of methylene chloride; 430 mg (1.37 mmol) of m-chloroperbenzoic acid are added and the reaction mixture is stirred for 4 h at RT. After extraction with water and 2N aqueous sodium hydroxide solution, the organic phase is dried and concentrated using a rotovapor. Chromatography (methylene chloride/methanol=19:1 to 9:1) and subsequent crystallisation (methylene chloride/diethyl ether) give N-[3-(1,1,2,2-tetrafluoro-ethoxy)-phenyl]-4-(N-oxido-4-pyridyl)-2-pyrimidineamine in the form of lemon-yellow crystals; FAB-MS: 381 (M+ +H), m.p. 191°-192°.

1. extractionAfter extraction with water and 2N aqueous sodium hydroxide solution
2. customthe organic phase is dried
3. concentrationconcentrated
4. customChromatography (methylene chloride/methanol=19:1 to 9:1) and subsequent crystallisation (methylene chloride/diethyl ether)