反応 #4384

ord-cd3f0cac90124ff0adb84e6417ad574b

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度cooling
  2. 2
    洗浄the mixture was washed with water
  3. 3
    乾燥dried over magnesium sulfate
  4. 4
    その他evaporated in vacuo
  5. 5
    その他The oily residue was purified by column chromatography on silica gel (60 g)

実験手順

Tosyl chloride (3.81 g) was added to a solution of 3-hydroxy-5-hexyn-2-one (2.24 g) and triethylamine (2.424 g) in methylene chloride (20 ml) under ice-cooling. After being stirred for 2.5 hours, the mixture was washed with water, dried over magnesium sulfate and evaporated in vacuo. The oily residue was purified by column chromatography on silica gel (60 g) using methylene chloride as an eluent to give an oil of 3-tosyloxy-5-hexyn-2-one (2.94 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04725601uspto-grants-1988_02