反应 #1269047

ord-80f8011300b24bbe992345955f08ebc5

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度while cooling on ice, extraction
  2. 2
    洗涤the extract was washed with brine
  3. 3
    干燥dried over magnesium sulfate
  4. 4
    workup.DISTILLATIONthe solvent was distilled off under reduced pressure

实验过程

Potassium tert-butoxide (11.1 g) was added to a solution of N-amino-2-(1-butynyl)-4-methoxypyridinium mesitylenesulfonate (20.7 g) in tetrahydrofuran (300 mL) and N,N-dimethylformamide (15 mL), and the mixture was stirred at room temperature for 1 hour. Water was added while cooling on ice, extraction was performed with ethyl acetate, the extract was washed with brine and dried over magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was subjected to silica gel column chromatography (200 g), and the title compound (6.44 g) was obtained from the n-hexane:ethyl acetate (3:1) fraction as a yellow oil.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07285666B2uspto-grants-2007_10