반응 #9284

반응 방정식

ethyl acetate

Potassium tert-butoxide

N-amino-2-(1-butynyl)-4-methoxypyridinium mesitylenesulfonate

Water

→

title compound

수율 66.5%

2-Ethyl-4-methoxypyrazolo[1,5-a]pyridine

수율 66.5%

용매

tetrahydrofuran

N,N-dimethylformamide

반응 조건

후처리

1. 1
   온도while cooling on ice, extraction
2. 2
   세척the extract was washed with brine
3. 3
   건조dried over magnesium sulfate
4. 4
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure

실험 절차

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.

출처