HRID1678065

反应详情

EQUATION

反应方程式

HRID 1678065 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe solids were removed by filtration
  2. washrinsed well with acetonitrile
  3. customThe solvent was removed in vacuo
  4. customthe residue partitioned between ether (50 mL) and water (25 mL)
  5. extractionThe aqueous phase was extracted with ether (2×25 mL)
  6. washwashed with brine
  7. dry with materialDried (Na2SO4)
  8. filtrationfiltered
  9. customsolvent removed in vacuo
  10. customaffording product as a pale yellow liquid, 19 g, 74 percent yield