反应详情

温度

0 °C

1.00 g (3.2 mmol) of 5-chloromethyl-4-cyclopropyl-2-(4-trifluoromethyl-phenyl)-pyrimidine (example 27F]) was dissolved in 20 ml of DMF. Then, the reaction mixture was cooled down to 0° C. 0.36 ml=0.366 g (3.52 mmol) of methyl-carbamic acid ethyl ester was added to the stirred solution, followed by 0.14 g (3.2 mmol) of sodium hydride (55%). After 18 hours, the reaction mixture was poured into crashed ice, the pH was adjusted to <3 with HCl/H2O and it was then extracted twice with Et2O. The combined organic phases were washed with water, dried over anhydrous magnesium sulfate and evaporated. The crude product was purified by flash chromatography (SiO2, gradient of EtOAc, n-heptane) to give 0.87 g of the title compound as light yellow solid.

1. additionthe reaction mixture was poured
2. extractionwas then extracted twice with Et2O
3. washThe combined organic phases were washed with water
4. dry with materialdried over anhydrous magnesium sulfate
5. customevaporated
6. customThe crude product was purified by flash chromatography (SiO2, gradient of EtOAc, n-heptane)