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Triethylamine → 1-Benzyl-3,5-dimethyl-1H-pyrazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Acetylacetone | HCID 31261 | — |
| 反応物 | Benzylhydrazine dihydrochloride | HCID 146540 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 1-Benzyl-3,5-dimethyl-1H-pyrazole | HCID 603765 | 92% |
反応手順
Dissolve 2,4-pentanedione (5.09 g, 50.8 mmol) and benzylhydrazine dihydrochloride (10.91 g, 55.9 mmol) in acetic acid (40 mL). Slowly add triethylamine (15.6 mL, 0.112 mol) and stir the mixture for 18 hr. Concentrate the solution then dilute the residue with saturated aqueous sodium bicarbonate and extract 3 times with ethyl acetate. Dry (sodium sulfate), filter, concentrate and purify (silica gel chromatography, eluting with 40:60 hexanes:ethyl acetate), to give 1-benzyl-3,5-dimethyl-1H-pyrazole as a yellow oil (8.703 g, 92%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08202873B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-adf012ae9ce445b39981d5845a2c7100 |
| 出典メモ | uspto-grants-2012_06 |