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Water → 1-Ethyl [2-oxo-3-(2-oxo-2-phenylethyl)cyclohexyl]acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Phenacyl bromide | HCID 6259 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-Ethyl [2-oxo-3-(2-oxo-2-phenylethyl)cyclohexyl]acetate | HCID 68858933 | 50% |
反応手順
Intermediate 2 (667 mg, 2.81 mmol) was dissolved in dimethylformamide (14 ml), 2-bromo-1-phenylethanone (560 mg, 2.81 mmol) was added and the reaction stirred for 24 h at room temperature. Water (5 ml) was added and the reaction allowed to stir for a further 24 h. The mixture was then diluted with ethyl acetate (100 ml) and washed with water. The aqueous fraction was re-extracted three times with ethyl acetate and the combined organic fractions washed three times with water, then dried over sodium sulfate, filtered and concentrated in vacuo. Column chromatography (10-20% ethyl acetate/hexanes) provided the title compound as a pale yellow oil (428 mg, 50%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07728022B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-6954c721ef9f486e9691b22e474bc1ae |
| 出典メモ | uspto-grants-2010_06 |