HRID1165695
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
The 5-cyclohexylmethylene-3-(2-fluorophenyl)-imidazolidine-2,4-dione (2.25 g, 7.81 mmol), cesium carbonate (2.6 g, 8.0 mmol) and methyl iodide (1.66 g, 11.7 mmol) were stirred overnight in DMF (25 mL). The solution was diluted with water and extracted with ethyl acetate (3×). The combined extracts were washed with brine (saturated, 2×), dried (over MgSO4), filtered and concentrated. Purification by column chromatography afforded 1.9 grams of 5-cyclohexylmethylene-3-(2-fluorophenyl)-1-methylimidazolidine-2,4-dione, a white solid, m.p. 131°-137° C.
WORKUP
后处理
- extractionextracted with ethyl acetate (3×)
- washThe combined extracts were washed with brine (saturated, 2×)
- dry with materialdried (over MgSO4)
- filtrationfiltered
- concentrationconcentrated
- customPurification by column chromatography