HRID1616610

反应详情

EQUATION

反应方程式

HRID 1616610 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Add a solution of LiOH (0.98 g, 40.86 mmol) in water (30 mL) to a rapidly stirred solution of 4-[5-(2-Methoxy-phenyl)-isoxazol-3-yl]-butyric acid methyl ester (2.25 g, 8.17 mmol) in dioxane (60 mL), stir at room temperature overnight Quench with 1N HCl solution and concentrate to remove the majority of the dioxane. Add 1N NaOH to adjust pH to 4-5, extract with EtOAc (×2). Dry combined organic layers over MgSO4 and concentrate to get 2.15 g yellow oil. Recrystallize from EtOAc/hexanes to afford the title compound (1.67 g, 78%). MS (IS) 262 (M+1)+.

WORKUP

后处理

  1. customQuench with 1N HCl solution
  2. concentrationconcentrate
  3. customto remove the majority of the dioxane
  4. additionAdd 1N NaOH
  5. extractionextract with EtOAc (×2)
  6. customDry
  7. concentrationconcentrate