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Methyl (5-fluoro-2-methyl-1H-inden-3-yl)acetate → 5-fluoro-2-methyl-1H-3-indenyl-(2-hydroxy) ethane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl (5-fluoro-2-methyl-1H-inden-3-yl)acetate | HCID 15434585 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-fluoro-2-methyl-1H-3-indenyl-(2-hydroxy) ethane | HCID 13933293 | 63% |
反応手順
To a solution of methyl 5-fluoro-2-methyl-3-indenyl- acetate (24 g) in dry THF (300 ml) lithiumaluminum hydride (6.9 g) is added. The mixture is stirred at room temperature for 1.5 hours. Excess LiA1H4 is destroyed with saturated aqueous NaHSO4 solution. The organic phase is concentrated in vacuo, and the crude product is purified via silica gel column chromatography elution with methylene chloride. The residue is recrystallized from hexane to give 5-fluoro-2-methyl-1H-3-indenyl-(2-hydroxy) ethane (yield 63%; m.p. 65-66.5° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05902827 |
| 出典データセット | uspto-grants-1999_05 |
| ORD ID | ord-d86fab6ae11c445a8ae1cf5d99ddf104 |
| 出典メモ | uspto-grants-1999_05 |