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Hydrochloric Acid → 1-(4'-Methoxyphenyl)-1,4-dihydro-indeno[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 | 4-Methoxyphenylhydrazine hydrochloride | HCID 2723904 | — |
| 反応物 | 1H-Inden-1-one, 2,3-dihydro-2-(hydroxymethylene)- | HCID 3764882 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-(4'-Methoxyphenyl)-1,4-dihydro-indeno[1,2-c] pyrazole | HCID 15319940 | — |
反応手順
2-Hydroxymethylene inden-l-one (Example 1(ii) (a) (4.0 g; 25 mmol), p-methoxyphenyl hydrazine hydrochloride (Aldrich) (4.41 g; 25.25 mmol), 10 M hydrochloric acid (1 cm3) and ethanol (30 cm3), were heated under reflux, for 21 hours. After cooling, the mixture was concentrated in vacuo and the residue dissolved in dichloromethane, then washed with 2M NaOH, dried, filtered and concentrated in vacuo. Purification by column chromatography [Eluant: (dichloromethane: ethanol: ammonia (200:8:1)] Kugelrohr distillation (170° C.; 0.02 mmHg) and recrystallisation (ethanol) afforded needle shaped crystals, m.p. 102-103° 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-2d264ec5b08e4c85957d76acb20b40b8 |
| 出典メモ | uspto-grants-2000_10 |