HRID870465

反应详情

EQUATION

反应方程式

HRID 870465 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Into a 50-mL round-bottom flask was placed ether (10 mL), CH3CN (5 mL) and 2-(2-ethylphenyl)ethan-1-ol (900 mg, 5.99 mmol, 1.00 equiv). Then imidazole (570 mg, 8.38 mmol, 1.40 equiv), PPh3 (2.20 g, 8.39 mmol, 1.40 equiv) and I2 (1.98 g, 7.80 mmol, 1.30 equiv) were added at 0° C. The resulting solution was stirred for 6 h at room temperature. The reaction was then quenched by the addition of 10 mL of saturated Na2SO3 solution. The resulting solution was extracted with 3×50 mL of ethyl acetate and the organic layers combined, dried over Na2SO4 and concentrated under vacuum. The residue was applied onto a silica gel column with ethyl acetate/petroleum ether (1:20). Purification afforded 1.16 g (74%) of 1-ethyl-2-(2-iodoethyl)benzene as a colorless oil.

WORKUP

后处理

  1. customInto a 50-mL round-bottom flask was placed
  2. customThe reaction was then quenched by the addition of 10 mL of saturated Na2SO3 solution
  3. extractionThe resulting solution was extracted with 3×50 mL of ethyl acetate
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated under vacuum
  6. customPurification