HRID1532854

反应详情

EQUATION

反应方程式

HRID 1532854 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of thionyl chloride (10.0 g, 84.0 mmol) in DMF (10 mL) was added dropwise to a solution of 4-hydroxymethyl-2-phenylbenzoic acid, methyl ester (12.1 g, 50 mmol), prepared as in Example 158C, and LiCl (2.33 g, 55.0 mmol) in DMF (40 mL). After 1 hour, the reaction mixture was poured into H2O and the resulting mixture was extracted with ether (3×). The combined organic extracts were rinsed with H2O (2×), saturated aqueous NaHCO3 (3×) and brine, dried (MgSO4) and concentrated under reduced pressure to provide the desired compound (10.8 g, 83%) as a clear, colorless oil.

WORKUP

后处理

  1. extractionthe resulting mixture was extracted with ether (3×)
  2. washThe combined organic extracts were rinsed with H2O (2×), saturated aqueous NaHCO3 (3×) and brine
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated under reduced pressure