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m-Chloroperbenzoic acid → 5,6,7,8-Tetrahydroquinolin-5-one N-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 5(6H)-Quinolinone, 7,8-dihydro- | HCID 3016811 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5,6,7,8-Tetrahydroquinolin-5-one N-oxide | HCID 117899564 | 83.7% |
反応手順
5,6,7,8-Tetrahydroquinolin-5-one (7.12 g) was dissolved in dichloromethane (138 mL), added with 3-chloroperbenzoic acid (14.5 g) under ice cooling, and stirred for 4 hours at the same temperature. After adding a saturated aqueous solution of sodium hydrogen carbonate and diluting with chloroform, insoluble was removed by filtration through Celite. After adding 1 mol/L aqueous solution of sodium hydroxide, it was extracted with chloroform and dried over anhydrous sodium sulfate. The solvent was then evaporated under reduced pressure. The residues were suspended in diethyl ether and collected by filtration to obtain the title compound (6.61 g) as a yellow powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09290440B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-3520671ade864827b17cbe7923004bab |
| 出典メモ | uspto-grants-2016_03 |