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Hexane → 9-Methylene-9H-fluorene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Fluorenone | HCID 10241 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 触媒 | Methyltriphenyliphosphonium bromide | HCID 74505 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 9-Methylene-9H-fluorene | HCID 78147 | 76.3% |
反応手順
A suspension of methyl triphenylphosphonium bromide (31.22 g; 87.3 mmol) in 500 mL of ether was added at -30° C. 10M n-butyllithium in hexane (8.73 mL; 87.3 mmol) and the mixture was allowed to stir at room temperature for 1/2 h. To the above mixture was added 15 g (83.2 mmol) of 9-fluorenone in 50 mL of tetrahydrofuran and the mixture was refluxed for 1 h. The above mixture was cooled to 0° C., filtered, and concentrated to yield 11.3 g (76.3%) of 9-methylene-fluorene (Formula III: R3 =R4 =H; R5 =R6 together form a 9-fluorene ring).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05554620 |
| 出典データセット | uspto-grants-1996_09 |
| ORD ID | ord-898a58f2a809496f93f0a2a98eaea946 |
| 出典メモ | uspto-grants-1996_09 |