HRID1789653
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 8.28 g (47.52 mmol) of 4-fluorophenyl methyl sulfone dissloved in 20 mL DMF was added 5.20 g (57.03 mmol) of 2-(methylthio)ethyl amine (1.2 eq.), followed by 13.13 g (95.04 mmol, 2 eq.) potassium carbonate. The mixture was heated to 65° C. and stirred for 12 h. Upon cooling to room temperature, the mixture was partitioned between EtOAc and brine, dried over MgSO4 and concentrated. Column chromatography, eluting with ethyl acetate/hexane, provided 5.53 g of 4-[2-(methylthio)ethylamino]phenyl methyl sulfone, pure by 1H NMR.
WORKUP
后处理
- temperatureUpon cooling to room temperature
- customthe mixture was partitioned between EtOAc and brine
- dry with materialdried over MgSO4
- concentrationconcentrated
- washColumn chromatography, eluting with ethyl acetate/hexane