反応 #9276

反応方程式

N-amino-2-(1-butynyl)pyridinium mesitylenesulfonate

potassium tert-butoxide

→

title compound

2-Ethylpyrazolo[1,5-a]pyridine

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   抽出to the reaction mixture, extraction
2. 2
   抽出The aqueous layer was again extracted with ethyl acetate
3. 3
   ろ過the insoluble portion was filtered with a celite
4. 4
   ろ過filter
5. 5
   洗浄washed with brine
6. 6
   乾燥After drying over anhydrous magnesium sulfate and filtration
7. 7
   濃縮the solvent was concentrated under reduced pressure
8. 8
   その他the residue was purified by silica gel column chromatography

実験手順

A 6.1 g portion of the obtained N-amino-2-(1-butynyl)pyridinium mesitylenesulfonate was dissolved in tetrahydrofuran (600 mL), potassium tert-butoxide (3.55 g) was added at room temperature, and the mixture was vigorously stirred for 30 minutes. After adding ice water to the reaction mixture, extraction was performed with ethyl acetate. The aqueous layer was again extracted with ethyl acetate, the insoluble portion was filtered with a celite filter, and the organic layers were combined and washed with brine. After drying over anhydrous magnesium sulfate and filtration, the solvent was concentrated under reduced pressure, the residue was purified by silica gel column chromatography, and the title compound (0.63 g) was obtained from the n-hexane:ethyl acetate (10:1) fraction as a light yellow oil.

出典