반응 #9295

반응 방정식

Water

Sodium triacetoxyborohydride

[7-(2,4-dichlorophenyl)-2-ethylpyrazolo[1,5-a]pyridin-3-yl]amine

sodium sulfate

→

title compound

수율 109.8%

N-[7-(2,4-Dichlorophenyl)-2-ethylpyrazolo[1,5-a]pyridin-3-yl]-N-(3-hexyl)amine

수율 109.8%

용매

ethyl acetate

acetic acid

3-hexanone

반응 조건

후처리

1. 1
   workup.ADDITIONwere added
2. 2
   workup.STIRRINGstirring
3. 3
   workup.WAITwas continued for 2 hours
4. 4
   세척the extract was washed with saturated aqueous sodium hydrogencarbonate and brine
5. 5
   건조After drying the obtained organic layer over anhydrous magnesium sulfate
6. 6
   여과filtering it
7. 7
   농축the solvent was concentrated under reduced pressure
8. 8
   기타the residue was purified by silica gel column chromatography

실험 절차

After dissolving [7-(2,4-dichlorophenyl)-2-ethylpyrazolo[1,5-a]pyridin-3-yl]amine (30 mg) in acetic acid (1 mL), 3-hexanone (0.024 mL) and sodium sulfate (139 mg) were added and the mixture was stirred at room temperature for 30 minutes. Sodium triacetoxyborohydride (41.5 mg) was then added, and stirring was continued for 2 hours. Water was added to the reaction mixture, extraction was performed with ethyl acetate and the extract was washed with saturated aqueous sodium hydrogencarbonate and brine. After drying the obtained organic layer over anhydrous magnesium sulfate and filtering it, the solvent was concentrated under reduced pressure, the residue was purified by silica gel column chromatography, and the title compound (21 mg) was obtained from the n-hexane:ethyl acetate (30:1) fraction as a yellow oil.

출처