HRID625697

反应详情

EQUATION

反应方程式

HRID 625697 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methyl 3-(2-bromo-3,5-difluorophenyl)propanoate (prepared as described in Step 1, 4.3 g) in aqueous NaOH (4 M, 13.5 mL) and 2-propanol (30 mL) is heated at 50° C. for 2 hours. Water is added, the mixture washed with diethyl ether, acidified to ca. pH 5 by adding concentrated aqueous HCl, and extracted twice with diethyl ether. The combined extracts of the acidified mixture are washed with brine and volatiles evaporated under reduced pressure. The resulting material (Yield 3.6 g) is used in the next step without further purification. LC (METHOD 7): tR=0.99 min.

WORKUP

后处理

  1. washthe mixture washed with diethyl ether
  2. additionby adding concentrated aqueous HCl
  3. extractionextracted twice with diethyl ether
  4. washThe combined extracts of the acidified mixture are washed with brine and volatiles
  5. customevaporated under reduced pressure
  6. customThe resulting material (Yield 3.6 g) is used in the next step without further purification