HRID1798566

反应详情

EQUATION

反应方程式

HRID 1798566 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-(4-(1H-pyrazol-1-yl)phenyl)-2-methoxyacetate (0.204 g, 0.83 mmol) in dry MeOH (5 mL) under argon was added a solution of KOH in MeOH (1.6 mL of a 0.5 M solution, 8.3 mmol) and the reaction was heated to reflux for 5 hours. The reaction mixture was cooled to room temperature and the volatiles were removed under reduced pressure. The residue was diluted with saturated aqueous NH4Cl and extracted with EtOAc. Additional EtOAc was then used to extract the aqueous phase as the pH was adjusted from ˜8 to ˜2 using concentrated HCl. The combined organics were dried over Na2SO4, filtered, and the solvents removed under reduced pressure to yield 2-(4-(1H-pyrazol-1-yl)phenyl)-2-methoxyacetic acid (0.18 g, 95%) which was used without further purification.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 5 hours
  3. customthe volatiles were removed under reduced pressure
  4. additionThe residue was diluted with saturated aqueous NH4Cl
  5. extractionextracted with EtOAc
  6. extractionto extract the aqueous phase as the pH
  7. dry with materialThe combined organics were dried over Na2SO4
  8. filtrationfiltered
  9. customthe solvents removed under reduced pressure