HRID748903

反应详情

EQUATION

反应方程式

HRID 748903 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Combine 4-bromo-2-fluoro-1-methylsulfanyl-benzene (4.8 g, 22 mmol) and sodium methanethiolate (1.6 g, 22 mmol) in DMF (50 mL). Stir for 48 hours. Pour the reaction mixture into ice (10 g). Separate the layers and wash the organic layer with aqueous saturated NaHCO3 and brine. Dry with MgSO4, filter and concentrate in vacuo. Chromatograph the residue on a column eluting with diethyl ether in hexane (0 to 5%) to give 4.82 g of 4-bromo-1,2-bis-methylsulfanylbenzene (89%).

WORKUP

后处理

  1. customSeparate the layers
  2. washwash the organic layer with aqueous saturated NaHCO3 and brine
  3. dry with materialDry with MgSO4
  4. filtrationfilter
  5. concentrationconcentrate in vacuo
  6. washChromatograph the residue on a column eluting with diethyl ether in hexane (0 to 5%)