反应详情

温度

100 °C

The mixture of 6-amino-5-(trifluoromethyl)pyrimidin-4-ol (N-4) (300 mg, 1.66 mmol) in POCl3 (8 mL) in a pressure vessel is stirred at 100° C. for 1 h. The mixture is allowed to cool to RT and concentrated in vacuo. The residue is taken up in water (20 mL), basified with saturated NaHCO3 aqueous solution to pH=9 and then extracted with DCM (30 mL×3). The combined organic layers are washed with brine, dried over Na2SO4 and filtered. The filtrate is concentrated in vacuo to afford the desired product, 6-chloro-5-(trifluoromethyl)pyrimidin-4-amine (N-5) as a yellow solid.

1. temperatureto cool to RT
2. concentrationconcentrated in vacuo
3. extractionextracted with DCM (30 mL×3)
4. washThe combined organic layers are washed with brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationThe filtrate is concentrated in vacuo