HRID1105617

反应详情

EQUATION

反应方程式

HRID 1105617 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Fluoromethyl-2-phthalimido-5-methoxy-valeronitrile (1.20 g, 4.14 mmol), trimethylsilyl iodide (3.2 g, 16 mmol) and chloroform (15 mL) are heated to 60° C. under nitrogen for 48 hours. After removal of the solvent, the residue is dissolved in chloroform, washed with water, sodium thiosulfate solution and water again, dried and evaporated to give the crude product as an oil (1.2 g). This is purified by chromatography on silica (ethyl acetate/petroleum ether 1:3) to give pure 2-fluoromethyl-2-phthalimido-5-iodo-valeronitrile.

WORKUP

后处理

  1. customAfter removal of the solvent
  2. dissolutionthe residue is dissolved in chloroform
  3. washwashed with water, sodium thiosulfate solution and water again
  4. customdried
  5. customevaporated
  6. customto give the crude product as an oil (1.2 g)
  7. customThis is purified by chromatography on silica (ethyl acetate/petroleum ether 1:3)