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Triethylamine → 3-tert-Butyl-1-(3,4-dimethylphenyl)-1H-pyrazol-5-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Pentanenitrile, 4,4-dimethyl-3-oxo- | HCID 108871 | — |
| 反応物 | 1-(3,4-Dimethylphenyl)hydrazine hydrochloride | HCID 173740 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 3-tert-Butyl-1-(3,4-dimethylphenyl)-1H-pyrazol-5-amine | HCID 10868500 | 66.9% |
反応手順
To a solution of pivaloylacetonitrile (400 mg) in toluene (10 mL) were added 3,4-dimethylphenylhydrazine hydrochloride (520 mg) and triethylamine (0.4 mL) and refluxed with heating for 5 hours. The reaction mixture was added with a saturated sodium hydrogen carbonate aqueous solution. The obtained organic layer was washed with a saturated sodium chloride aqueous solution. The obtained organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The obtained residue was purified on silica gel column chromatography (hexane:ethyl acetate=4:1) to give the titled compound (490 mg) having the following physical data.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09242977B2 |
| 出典データセット | uspto-grants-2016_01 |
| ORD ID | ord-c103ebe0bf7f4f7eb4213ff3e0bbd809 |
| 出典メモ | uspto-grants-2016_01 |