HRID2183644

反应详情

EQUATION

反应方程式

HRID 2183644 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-(4-chlorobenzo[b]thiophen-2-yl)butan-1-one (0.93 g), phenyltrimethylammonium tribromide (1.47 g) and tetrahydrofuran (20 ml) was stirred under nitrogen at ambient temperature for 66 hours, then it was filtered and diluted with water (50 ml). The product was extracted into dichloromethane (3×30 ml), the combined extracts were dried (MgSO4) and the solvents were removed in vacuo. The residue was purified by flash chromatography over silica using dichloromethane as eluant. Appropriate fractions were combined and the solvents removed in vacuo to leave 2-bromo-1-(4-chlorobenzo[b]thiophen-2-yl)butan-1-one (1.07 g) which was used without further purification.

WORKUP

后处理

  1. filtrationit was filtered
  2. additiondiluted with water (50 ml)
  3. extractionThe product was extracted into dichloromethane (3×30 ml)
  4. dry with materialthe combined extracts were dried (MgSO4)
  5. customthe solvents were removed in vacuo
  6. customThe residue was purified by flash chromatography over silica
  7. customthe solvents removed in vacuo