関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzoylacetonitrile | HCID 64799 | — |
| 反応物 | o-Tolylhydrazinium(1+) chloride | HCID 71554 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1-(2-methylphenyl)-3-phenyl-1H-pyrazol-5-amine | HCID 12049974 | 45.7% |
反応手順
Benzoylacetonitrile (500 mg, 3.44 mmol) and o-tolylhydrazine hydrochloride (574 mg, 3.61 mmol) were placed in a microwave vial and dissolved in methanol (1.7 mL). The reaction vessel was sealed, placed in a microwave oven and heated at 120° C. for 1 hour. After this period, the reaction mixture was concentrated onto silica gel and purified by flash chromatography (0-50% ethyl acetate/hexanes gradient) to afford the desired intermediate, 5-phenyl-2-o-tolyl-2H-pyrazol-3-ylamine (392 mg). LC/MS: Calc. C16H15N3 249.13 amu; Obs. [M+H]+=250.2 amu.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09447058B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
|---|
| ORD ID | ord-463d2c9fe0064459b0b0a809e8778bb7 |
|---|
| 出典メモ | uspto-grants-2016_09 |
|---|