HRID748697

反应详情

EQUATION

反应方程式

HRID 748697 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The 5-[(4-chlorophenyl)sulfonyl]-5-(2,5-difluorophenyl)-4-methyl-1-pentanol (170 mg, 0.437 mmol) obtained in Example 40 and carbon tetrabromide (170 mg, 0.648 mmol) were dissolved in methylene chloride (8 ml). While stirring under ice cooling, triphenylphosphine (135 mg, 0.515 mmol) was added to the resulting solution, followed by stirring at room temperature for 14 hours. To the reaction mixture were added carbon tetrabromide (170 mg, 0.437 mmol) and triphenylphosphine (135 mg, 0.515 mmol) under ice cooling. The reaction mixture was stirred at room temperature for 6 hours. The residue obtained by concentrating the reaction mixture under reduced pressure was purified by silica gel chromatography (hexane:ethyl acetate=10:1), whereby the title compound (192 mg, 97%) was obtained as a colorless oil.

WORKUP

后处理

  1. stirringby stirring at room temperature for 14 hours
  2. stirringThe reaction mixture was stirred at room temperature for 6 hours
  3. customThe residue obtained
  4. concentrationby concentrating the reaction mixture under reduced pressure
  5. customwas purified by silica gel chromatography (hexane:ethyl acetate=10:1), whereby the title compound (192 mg, 97%)
  6. customwas obtained as a colorless oil