HRID1678065
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
A mechanically stirred slurry of 5-bromo-2-(methanesulfonyl)pyrimidine (24 g, 0.10 mol), trifluoroethanol (15 g, 0.15 mol), and potassium carbonate (28 g, 0.20 mol) in acetonitrile (250 mL) was heated at 70° C. for 12 hours. HPLC analysis indicated complete conversion. The solids were removed by filtration, and rinsed well with acetonitrile. The solvent was removed in vacuo and the residue partitioned between ether (50 mL) and water (25 mL). The aqueous phase was extracted with ether (2×25 mL), the organic layers combined, and washed with brine. Dried (Na2SO4), filtered, and solvent removed in vacuo, affording product as a pale yellow liquid, 19 g, 74 percent yield.
WORKUP
后处理
- customThe solids were removed by filtration
- washrinsed well with acetonitrile
- customThe solvent was removed in vacuo
- customthe residue partitioned between ether (50 mL) and water (25 mL)
- extractionThe aqueous phase was extracted with ether (2×25 mL)
- washwashed with brine
- dry with materialDried (Na2SO4)
- filtrationfiltered
- customsolvent removed in vacuo
- customaffording product as a pale yellow liquid, 19 g, 74 percent yield