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Hydrochloric Acid → 1,4-Dihydro-1-phenylindeno[1,2-c]pyrazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Phenylhydrazine hydrochloride | HCID 60962 | — |
| 反応物 | 1H-Inden-1-one, 2,3-dihydro-2-(hydroxymethylene)- | HCID 3764882 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1,4-Dihydro-1-phenylindeno[1,2-c]pyrazole | HCID 10879009 | — |
反応手順
2-Hydroxymethlene indan-1-one (Example 1(ii)(a) (6.0 g, 37.5 mmol), phenylhydrazine hydrochloride (Aldrich) (5.48 g, 37.9 mmol), 10 M hydrochloric acid (1 cm3) and ethanol (30 cm3) were stirred under reflux for 19 hours. After cooling, the solvent was evaporated under reduced pressure and the residue dissolved in dichloromethane, then washed with 2M sodium hydroxide. The organic layer was separated, dried (Na2SO4) filtered and concentrated in vacuo. Purification by Kugelrohr distillation afforded an off-white solid (150° C., 0.01 mmHg) m.p. 119-120° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06130228 |
| 出典データセット | uspto-grants-2000_10 |
| ORD ID | ord-380d35a1d5e1462b8e71bdae12a790df |
| 出典メモ | uspto-grants-2000_10 |