HRID705433
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 methyl 2-(bromomethyl)-4-methoxybenzoate (960 mg, 3.7 mmol) in DCM (18.5 mL) was added morpholine (0.68 mL, 7.8 mmol). The reaction mixture was stirred at room temperature overnight and poured onto iced water. The aqueous mixture was extracted with DCM (3×), and the combined organics were dried over MgSO4, filtered, and concentrated in vacuo to provide a yellow oil. The crude material was purified by flash chromatography on silica using a gradient of EtOAc in hexane (0 to 50%) as eluant. The tittle product was obtained as a clear oil (490 mg, 50%)
WORKUP
后处理
- extractionThe aqueous mixture was extracted with DCM (3×)
- dry with materialthe combined organics were dried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customto provide a yellow oil
- customThe crude material was purified by flash chromatography on silica using a gradient of EtOAc in hexane (0 to 50%) as eluant