HRID1046296

反应详情

EQUATION

反应方程式

HRID 1046296 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2,2,3,3,4,4,4-heptafluorobutanol (5.7 g, 28.5 mmol) in DMF (100 mL) was stirred and cooled to −5° C. as sodium hydride (0.72 g, 30 mmol) was added. After 1 h at −5° C., the reaction was treated with 4-fluoronitrobenzene (4.1 g, 29 mmol). The reaction was allowed to warm to ambient temperature, concentrated, and slurried in methylene chloride (200 mL). The slurry was washed with an 1 N aqueous potassium hydroxide solution (2×) and brine solution, dried over basic alumina, treated with charcoal, filtered, and concentrated to give 4-(2′,2′,3′,3′,4′,4′,4′-heptafluorobutanoxy)nitrobenzene.

WORKUP

后处理

  1. additionwas added
  2. concentrationconcentrated
  3. washThe slurry was washed with an 1 N aqueous potassium hydroxide solution (2×) and brine solution
  4. customdried over basic alumina
  5. additiontreated with charcoal
  6. filtrationfiltered
  7. concentrationconcentrated