HRID1995493

反应详情

EQUATION

反应方程式

HRID 1995493 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 0.52 grams (0.005 mole) of 4,4-dimethyl-3-isoxazolidinone, 1.0 gram (0.005 mole) of (2-chloro-4-fluorophenyl)methyl bromide and 0.62 gram (0.005 mole) of potassium carbonate in 40 ml of dimethylformamide was stirred at ambient temperature for 18 hours. The dimethylformamide was removed under high vacuum with mild heat. The residue was extracted with methylene chloride. The extract was filtered and dried with sodium sulfate. The mixture was refiltered and the filtrate concentrated under reduced pressure to give an oil residue. The residue was slurried in warm hexane and a solid was removed by filtration. The filtrate was concentrated under reduced pressure to give 0.39 gram of 2-[(2-chloro-4-fluorophenyl)methyl]-4,4-dimethyl-3-isoxazolidinone as an oil.

WORKUP

后处理

  1. customThe dimethylformamide was removed under high vacuum with mild heat
  2. extractionThe residue was extracted with methylene chloride
  3. filtrationThe extract was filtered
  4. dry with materialdried with sodium sulfate
  5. concentrationthe filtrate concentrated under reduced pressure
  6. customto give an oil residue
  7. customa solid was removed by filtration
  8. concentrationThe filtrate was concentrated under reduced pressure