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
PROCEDURE
实验过程
To a solution of 3.06 g (14.23 mmol) of the product of Step B dissolved in 25 mL of anhydrous DMF was added 4.87 g (15.0 mmol) of cesium carbonate and the reaction mixture was magnetically stirred under a nitrogen atmosphere at room temperature for 15 minutes. Methyl α-bromo-3,4-methylenedioxyphenylacetate (4.08 g, 15.0 mmol) was then added and the reaction mixture was stirred for an additional 3 hours. The reaction mixture was then partitioned between EtOAc (80 mL) and 10% aqueous citric acid (300 mL). The organic layer was separated, washed with saturated aqueous NaHCO3, saturated aqueous NaCl, dried (MgSO4), filtered and evaporated. The residue was dried in vacuo to afford 5.90 g (5.79 theoretical) of the title compound which was used in the next step without further purification.
WORKUP
后处理
- stirringthe reaction mixture was stirred for an additional 3 hours
- customThe reaction mixture was then partitioned between EtOAc (80 mL) and 10% aqueous citric acid (300 mL)
- customThe organic layer was separated
- washwashed with saturated aqueous NaHCO3, saturated aqueous NaCl
- dry with materialdried (MgSO4)
- filtrationfiltered
- customevaporated
- customThe residue was dried in vacuo