Potassium Carbonate → HCID 21445403, compound

Temperature

40 °C

A mixture of 2-dimethylamino-4-trifluoromethyl-6-hydroxypyrimidine (3.1 G), anhydrous potassium carbonate (2.8 g), and dry ethyl acetate (50 ml) was refluxed together for 1 hour and then cooled to about 40° C. Diethylphosphorochloridate (2.54 g) was then added dropwise to the stirred mixture and when the addition was complete the mixture was refluxed for 16 hours, after which it was allowed to cool to the ambient temperature. After filtration to remove the solids present, the filtrate was washed with water (2 × 50 ml), 10% w/v aqueous sodium hydroxide solution (1 × 50 ml), and finally with water until the washings were neutral. The ethyl acetate solution was dried over anhydrous magnesium sulphate, and after filtering, the the solvent was evaporated under reduced pressure to yield a residual pale yellow oil, which on cooling and scratching yielded crystalline O,O-diethyl 2-dimethylamino-4-trifluoromethylpyrimidin-6-yl phosphate, melting point 22°-24° C.

1. temperaturewas refluxed together for 1 hour
2. additionthe addition
3. temperaturewas refluxed for 16 hours
4. temperatureto cool to the ambient temperature
5. filtrationAfter filtration
6. customto remove the solids present
7. washthe filtrate was washed with water (2 × 50 ml), 10%
8. dry with materialThe ethyl acetate solution was dried over anhydrous magnesium sulphate
9. filtrationafter filtering
10. customthe the solvent was evaporated under reduced pressure
11. customto yield a residual pale yellow oil, which
12. temperatureon cooling

ORD record

ord-f59d8bcb30ac48df8a7aba5161106cfe

Source dataset

uspto-grants-1977_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04014882