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Acetic Acid → 2-Methylfluorene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Fluorene-2-carboxaldehyde | HCID 34804 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Palladium hydroxide | HCID 9942167 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-Methylfluorene | HCID 15026 | 69.1% |
反応手順
A solution of 2-fluorenecarboxaldehyde (15 g, 77.1 mmol) in 250 mL of 10% solution of acetic acid in ethyl acetate was hydrogenated at 80 psi of hydrogen during 24 hours at room temperature over 20% palladium hydroxide on carbon (catalytic amount). The reaction was monitored by TLC (silica, 25% ethyl acetate in hexane). The catalyst was filtered off, evaporation of the solvents followed by recrystallization of the residual solid from ethanol:water 5:1 afforded 9.6 g (69.0%) of the product as colorless solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05079260 |
| 出典データセット | uspto-grants-1992_01 |
| ORD ID | ord-8f6e1c3af9924fbfa04f62eb84f9198e |
| 出典メモ | uspto-grants-1992_01 |