HRID479133

反应详情

EQUATION

反应方程式

HRID 479133 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7.33 g of the above prepared [5-methyl-2-(4-trifluoromethyl-phenyl)-oxazol-4-yl]-acetic acid (25.7 mmol) was dissolved in 120 ml of abs. THF and treated at 0° C. with 64 ml 1M BH3THF (2.5 eq.). The reaction mixture was then kept over night et ambient temperature. Careful quenching with MeOH and ice, twofold extraction with AcOEt, washing with water and brine, drying over magnesium sulfate, and evaporation of the solvents left a crude product which was refluxed for 30 min. in MeOH to liberate quantitatively the free alcohol. Flash chromatography (SiO2, hexane/AcOEt=7/3) delivered finally 6.38 g of the title compound as off-white crystals.

WORKUP

后处理

  1. dissolutionwas dissolved in 120 ml of abs
  2. waitThe reaction mixture was then kept over night
  3. customet ambient temperature
  4. customCareful quenching with MeOH and ice, twofold extraction with AcOEt
  5. washwashing with water and brine
  6. dry with materialdrying over magnesium sulfate, and evaporation of the solvents
  7. waitleft a crude product which
  8. temperaturewas refluxed for 30 min. in MeOH