反応 #2254218

反応方程式

[9-(prop-2-en-1-yl)-6-oxaspiro[4.5]decan-9-yl]hydrazine

Et3N

3-dimethylaminoacrolein

→

1-[9-(prop-2-en-1-yl)-6-oxaspiro[4.5]decan-9-yl]-1H-pyrazole

収率 31.0%

溶媒

i-PrOH

反応条件

後処理

1. 1
   温度The solution was refluxed for 3 h
2. 2
   その他The solvent removed
3. 3
   その他the residue was purified on 25 g Biotage snap column
4. 4
   洗浄eluted with 0-18% EtOAc in Hex (12CV)

実験手順

A solution of [9-(prop-2-en-1-yl)-6-oxaspiro[4.5]decan-9-yl]hydrazine (250 mg, 1.0 mmol) in 4 mL of i-PrOH were added Et3N and 3-dimethylaminoacrolein. The solution was refluxed for 3 h and then at 50° C. for 2 d. The solvent removed and the residue was purified on 25 g Biotage snap column, eluted with 0-18% EtOAc in Hex (12CV) to give 1-[9-(prop-2-en-1-yl)-6-oxaspiro[4.5]decan-9-yl]-1H-pyrazole (80 mg, 31% yield).

出典