HRID2068464

反应详情

EQUATION

反应方程式

HRID 2068464 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of C4F9I (0.96 mL, 5.6 mmol) was added dropwise over 10 min to a stirred mixture of 2,5-diiodo-p-xylene (0.5 g, 1.4 mmol), copper powder (1.4 g, 22.4 mmol) in DMSO (10 mL) at 130° C. The reaction mixture was subsequently stirred for a further 24 h at this temperature. After cooling to room temperature, it was poured into a beaker containing dichloromethane (30 mL) and water (30 mL). After filtering, the organic layer was separated, washed with water (3×30 mL), and dried over MgSO4. The residue was purified by column chromatography (hexane as eluent) to give the product 28 as a white solid (553 mg, 73%).

WORKUP

后处理

  1. additionit was poured into a beaker
  2. filtrationAfter filtering
  3. customthe organic layer was separated
  4. washwashed with water (3×30 mL)
  5. dry with materialdried over MgSO4
  6. customThe residue was purified by column chromatography (hexane as eluent)