反応 #9310

反応方程式

Water

cyclopropylmethyl bromide

N-[7-(2-methoxy-4,6-dimethylphenyl)-2-(methylsulfanyl)pyrazolo[1,5-a]pyridin-3-yl]-N-(2-oxetanylmethyl)amine

sodium hydride

→

title compound

N-Cyclopropylmethyl-N-[7-(2-methoxy-4,6-dimethylphenyl)-2-(methylsulfanyl)pyrazolo[1,5-a]pyridin-3-yl]-N-(2-oxetanylmethyl)amine

溶媒

ethyl acetate

N,N-dimethylformamide

反応条件

後処理

1. 1
   workup.ADDITIONwas added
2. 2
   温度while cooling on ice
3. 3
   洗浄the extract was washed with brine
4. 4
   乾燥After drying over anhydrous magnesium sulfate and filtration
5. 5
   濃縮the solvent was concentrated under reduced pressure
6. 6
   その他the residue was purified by silica gel column chromatography

実験手順

After dissolving N-[7-(2-methoxy-4,6-dimethylphenyl)-2-(methylsulfanyl)pyrazolo[1,5-a]pyridin-3-yl]-N-(2-oxetanylmethyl)amine (8 mg) in N,N-dimethylformamide (2 mL), sodium hydride (60%, 1.6 mg) was added while cooling on ice, and then cyclopropylmethyl bromide (3.8 μL) was added and the mixture was stirred at room temperature for 12 hours. Water was added to the reaction mixture, extraction was performed with ethyl acetate and the extract was 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 (1.8 mg) was obtained from the n-hexane:ethyl acetate (10:1) fraction as a yellow oil.

出典