関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | 1-Indanone, 3-phenyl- | HCID 98146 | — |
| 反応物 | Lithium diisopropylamide | HCID 2724682 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Methylindanone | HCID 249262 | 22% |
反応手順
A 2 M solution of LDA (21 mL, 1.05 eq, from Aldrich) was added dropwise to 3-phenyl-1-indanone (8.33 g, 40.0 mmol) in THF (300 mL) at −78° C. After 1 h at this temperature, iodomethane (3.00 mL, 1.2 eq) was added. The mixture was stirred at −78° C. for 2 h, at 0° C. for 30 min and quenched with sat NH4Cl (100 mL). After evaporation of THF in vacuo, the aqueous residue was extracted with EtOAc (3×100 mL). The combined extracts were washed with brine (20 mL), dried (MgSO4) and concentrated. Silica gel chromatography (EtOAc-Hex, 5:95 then 7:93 then 10:90) gave the 2-methylindanone (1.93 g, 22%). MS Found: (M+H)+=223.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07592461B2 |
|---|
| 出典データセット | uspto-grants-2009_09 |
|---|
| ORD ID | ord-327d7b10928b47c39928a5da8eb300f7 |
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| 出典メモ | uspto-grants-2009_09 |
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