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Water → 4-Tert-butyl-2-(2-oxo-2-phenylethyl)-cyclohexanone
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 | 1-[4-(Tert-butyl)-1-cyclohexen-1-YL]pyrrolidine | HCID 107232 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-Tert-butyl-2-(2-oxo-2-phenylethyl)-cyclohexanone | HCID 12270341 | — |
反応手順
To a 250-mL round-bottomed flask containing 3.3 mL of 1-(4-tert-butylcyclohex-1-enyl) pyrrolidine was added 100 mL anhydrous DMF, under nitrogen. The flask was fitted with an addition funnel containing 2-bromoacetophenone (4.12 gm) in 35 mL anhydrous DMF, which was dripped into the enamine solution over 60 min. This solution was stirred at ambient temperature for 10 hr, then 90 mL water was added to the solution and it was stirred for another 11 hr, under nitrogen. The solution was then extracted twice with ethyl acetate and water, the organic layers combined and further washed with water (3×), dried over sodium sulfate, filtered and rotovapped down to give a yellow oil. The oil was purified by MPLC using 10% ethyl acetate/hexanes.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09216966B2 |
| 出典データセット | uspto-grants-2015_12 |
| ORD ID | ord-aef2f0db77e943c6a1fdacc4326457ab |
| 出典メモ | uspto-grants-2015_12 |