HRID545071

反应详情

EQUATION

反应方程式

HRID 545071 的结构方程式

PROCEDURE

实验过程

Heat a mixture of 5-nitro-3-trifluoromethyl-pyridin-2-ol (416 mg, 2.0 mmol) and phosphorus oxychloride (1 mL) at 85° C. for 18 hours. Cool the mixture and remove the volatiles by rotary evaporation. Dissolve the residue in EtOAc (15 mL) and wash with water (10 mL), saturated NaHCO3(aq) (10 mL) and brine (10 mL). Dry the organic extract over MgSO4 and remove the solvent under reduced pressure to yield the title compound.

WORKUP

后处理

  1. temperatureHeat
  2. temperatureCool the mixture
  3. customremove the volatiles
  4. customby rotary evaporation
  5. dissolutionDissolve the residue in EtOAc (15 mL)
  6. washwash with water (10 mL), saturated NaHCO3(aq) (10 mL) and brine (10 mL)
  7. customDry the
  8. extractionorganic extract over MgSO4
  9. customremove the solvent under reduced pressure