反应 #9284
ord-e725fe37874e4314be98d52b6aead169
反应方程式
反应物
试剂
无
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度while cooling on ice, extraction
- 2洗涤the extract was washed with brine
- 3干燥dried over magnesium sulfate
- 4workup.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.