반응 #9276

반응 방정식

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

potassium tert-butoxide

→

title compound

2-Ethylpyrazolo[1,5-a]pyridine

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   추출to the reaction mixture, extraction
2. 2
   추출The aqueous layer was again extracted with ethyl acetate
3. 3
   여과the insoluble portion was filtered with a celite
4. 4
   여과filter
5. 5
   세척washed with brine
6. 6
   건조After drying over anhydrous magnesium sulfate and filtration
7. 7
   농축the solvent was concentrated under reduced pressure
8. 8
   기타the residue was purified by silica gel column chromatography

실험 절차

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.

출처