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Hydrochloric Acid → 1-(4-Fluorophenyl)-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-Fluorophenylhydrazine hydrochloride | HCID 69981 | — |
| 反応物 | 1H-Inden-1-one, 2,3-dihydro-2-(hydroxymethylene)- | HCID 3764882 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-(4-Fluorophenyl)-1, 4-dihydro-indeno [1, 2-c] pyrazole | HCID 12291066 | — |
反応手順
2-Hydroxymethylene indan-1-one, (Example 1(ii) (a) (4.004 g; 250 mmol), p-fluorophenyl hydrazine hydrochloride (Aldrich) (4.106 g; 25.25 mmol) 10M hydrochloric acid (1 cm3) and ethanol (30 cm3), were heated under reflux for 19 hours. After cooling, the solvent was evaporated under reduced pressure, then taken up in dichloromethane and washed with 2M NaOH. The organic layer was separated, dried (Na2SO4), filtered and concentrated in vacuo. Purification by Kugelrohr distillation (140° C.; 0.01 mmHg) afforded a yellow solid, m.p. 104-105° 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-538bde8ff3034153b72fd8cf2836b91c |
| 出典メモ | uspto-grants-2000_10 |