HRID1789653

反应详情

EQUATION

反应方程式

HRID 1789653 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureUpon cooling to room temperature
  2. customthe mixture was partitioned between EtOAc and brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated
  5. washColumn chromatography, eluting with ethyl acetate/hexane