HRID1377716

反应详情

EQUATION

反应方程式

HRID 1377716 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of methyl 2-allyloxy-4-(1-tertbutyloxycarbonyl-4-piperidinyloxy)benzoate (2.50 g, 6.39 mmol) from Step 1 above in methanol (40 mL) was added 2N NaOH (15.9 mL, 31.9 mmol). The reaction mixture was refluxed for 30 minutes and cooled in a ice water bath. The solution was acidified with 5% citric acid and the solvent was evaporated under reduced pressure. The residue was dissolved in EtOAC and washed with water (2×75 mL). The organic layer was dried (MgSO4), filtered, and the solvent was evaporated under reduced pressure to give 2-allyloxy-4-(1-tertbutyloxycarbonyl-4-piperidinyloxy)benzoic acid as a white solid, which was used without further purification.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 30 minutes
  2. temperaturecooled in a ice water bath
  3. customthe solvent was evaporated under reduced pressure
  4. dissolutionThe residue was dissolved in EtOAC
  5. washwashed with water (2×75 mL)
  6. dry with materialThe organic layer was dried (MgSO4)
  7. filtrationfiltered
  8. customthe solvent was evaporated under reduced pressure