HRID410038

反应详情

EQUATION

反应方程式

HRID 410038 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

To a solution of methyl 4-(bromomethyl)-3-fluorobenzoate (18 g, 73 mmol) in MeOH (150 ml) was added the solution of NaCN (7.2 g, 146 mmol) in H2O (40 ml). The mixture was stirred at 65° C. for 5 hours. Most of MeOH was evaporated and additional water was added and extracted by EtOAc (200 ml×3), dried with anhydrous Na2SO4, filtered and evaporated to give the crude product. Purification by column chromatography (PE/EtOAc=50/1 to 10/1) gave the product (8 g, 63.8%).

WORKUP

后处理

  1. customMost of MeOH was evaporated
  2. additionadditional water was added
  3. extractionextracted by EtOAc (200 ml×3)
  4. dry with materialdried with anhydrous Na2SO4
  5. filtrationfiltered
  6. customevaporated
  7. customto give the crude product
  8. customPurification by column chromatography (PE/EtOAc=50/1 to 10/1)