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Triethylamine → 1-[9-(prop-2-en-1-yl)-6-oxaspiro[4.5]decan-9-yl]-1H-pyrazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-(Dimethylamino)-2-propenal | HCID 79125 | — |
| 反応物 | [9-(Prop-2-en-1-yl)-6-oxaspiro[4.5]decan-9-yl]hydrazine | HCID 68314598 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 1-[9-(prop-2-en-1-yl)-6-oxaspiro[4.5]decan-9-yl]-1H-pyrazole | HCID 68314165 | 31% |
反応手順
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 (12 CV) to give 1-[9-(prop-2-en-1-yl)-6-oxaspiro[4.5]decan-9-yl]-1H-pyrazole (80 mg, 31% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08835488B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-a605260e4fe14622971415496bbdd4f6 |
| 出典メモ | uspto-grants-2014_09 |