HRID2390556

反应详情

EQUATION

反应方程式

HRID 2390556 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-bromo-3-(bromomethyl)benzonitrile (0.95 g, 3.46 mmol) in DMF (13.40 ml) was added thiomorpholine (0.417 ml, 4.15 mmol) and potassium carbonate (0.573 g, 4.15 mmol). The reaction mixture was allowed to stir at RT overnight. The reaction mixture was poured onto water and extracted with EtOAc (×2). The organic extractions were combined, washed with brine (×3), dried (MgSO4) and evaporated to give a yellow oil. This was purified by flash silica chromatography (Biotage column) (eluent=25% ether/isohexane) to give the sub-title compound as a colourless oil. Yield: 0.951 g

WORKUP

后处理

  1. additionThe reaction mixture was poured onto water
  2. extractionextracted with EtOAc (×2)
  3. extractionThe organic extractions
  4. washwashed with brine (×3)
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. customto give a yellow oil
  8. customThis was purified by flash silica chromatography (Biotage column) (eluent=25% ether/isohexane)