HRID748965

反应详情

EQUATION

反应方程式

HRID 748965 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Add 5-bromo-2-fluoro-1,3-dimethyl-benzene (3.5 g, 17.2 mmol) to dimethylformamide (DMF, 30 mL) at ambient temperature followed by sodium thiomethoxide (1.32 g, 17.9 mmol). Heat at 50° C. for 8 hours and dilute with water (10 mL) and diethyl ether (100 mL). Separate the layers, wash the organics with brine, and dry with magnesium sulfate before concentrating to a residue. Chromatograph the residue on a SiO2 column eluting with diethyl ether (20%) in hexane to give 566 mg (14%) of 5-bromo-1,3-dimethyl-2-methylsulfanyl-benzene.

WORKUP

后处理

  1. customSeparate the layers
  2. washwash the organics with brine
  3. dry with materialdry with magnesium sulfate
  4. concentrationbefore concentrating to a residue
  5. washChromatograph the residue on a SiO2 column eluting with diethyl ether (20%) in hexane