反応 #9295

反応方程式

Water

Sodium triacetoxyborohydride

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

sodium sulfate

→

title compound

収率 109.8%

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

収率 109.8%

溶媒

ethyl acetate

acetic acid

3-hexanone

反応条件

後処理

1. 1
   workup.ADDITIONwere added
2. 2
   workup.STIRRINGstirring
3. 3
   workup.WAITwas continued for 2 hours
4. 4
   洗浄the extract was washed with saturated aqueous sodium hydrogencarbonate and brine
5. 5
   乾燥After drying the obtained organic layer over anhydrous magnesium sulfate
6. 6
   ろ過filtering it
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

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.

出典