HRID4755

反应详情

EQUATION

反应方程式

HRID 4755 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To one liter of 1M borane-tetrahydrofuran complex was added a solution of 100 g (0.33 mole) of 3-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]benzeneactic acid in 200 ml of tetrahydrofuran. The solution is refluxed for 16 hours under nitrogen. The solution is then refluxed with 400 ml of 6N hydrochloric acid until evolution of hydrogen is complete. The mixture is filtered and evaporated. The residue is refluxed with 500 ml of methanol containing 10 ml of concentrated hydrochloric acid until methyl borate is no longer evolved. The solution is evaporated, and the residue is distilled at 110°-115° (0.7 mm) to give 37 g of 2-{3-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]phenyl}ethanol.

WORKUP

后处理

  1. temperatureThe solution is refluxed for 16 hours under nitrogen
  2. filtrationThe mixture is filtered
  3. customevaporated
  4. temperatureThe residue is refluxed with 500 ml of methanol containing 10 ml of concentrated hydrochloric acid until methyl borate
  5. customThe solution is evaporated
  6. distillationthe residue is distilled at 110°-115° (0.7 mm)