反应详情

温度

100 °C

To a mixture of 6-Chloro-4,5-diaminopyrimidine (0.70 g, 4.84 mmol) and 3-chlorobenzoic acid (0.76 g, 4.84 mmol) in the flask was added phosphoryl chloride (40.0 mL), and the resulting mixture was stirred for 16 h at 100° C. The reaction mixture was evaporated to remove excess phosphoryl chloride, and the residue was added to water (20 mL). The precipitate was filtered and purified by flash chromatography (0 to 5% Methanol/DCM) to afford the title compound (1.28 g, 31%) as a yellow solid. LC/MS: Rt=1.59 min, ES+ 265.0 (FA standard).

1. customThe reaction mixture was evaporated
2. customto remove excess phosphoryl chloride
3. additionthe residue was added to water (20 mL)
4. filtrationThe precipitate was filtered
5. custompurified by flash chromatography (0 to 5% Methanol/DCM)