HRID2102990
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
- 130 °C
PROCEDURE
实验过程
A suspension of 4-benzyloxy-2,3-dimethyl-phenol (960 mg), 1-methanesulfonyloxymethyl-cyclopropanecarboxylic acid ethyl ester, prepared as in Step 1 (890 mg) and cesium carbonate (1.5 g) in DMF (20 mL) was stirred at 130 ° C for 6 h, and the mixture was partitioned between EtOAc and water. The organic layer was washed with water, dried over MgSO4 and evaporated. The residue was purified by silica gel column eluting with 10% EtOAc in hexane to give 0.78 g of 1-(4-benzyloxy-2,3-dimethyl-phenoxymethyl)-cyclopropanecarboxylic acid ethyl ester as a clear oil.
WORKUP
后处理
- customthe mixture was partitioned between EtOAc and water
- washThe organic layer was washed with water
- dry with materialdried over MgSO4
- customevaporated
- customThe residue was purified by silica gel column
- washeluting with 10% EtOAc in hexane