HRID410038
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customMost of MeOH was evaporated
- additionadditional water was added
- extractionextracted by EtOAc (200 ml×3)
- dry with materialdried with anhydrous Na2SO4
- filtrationfiltered
- customevaporated
- customto give the crude product
- customPurification by column chromatography (PE/EtOAc=50/1 to 10/1)