関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 反応物 | 4-Methoxy-2-methylquinoline | HCID 15560678 | — |
| 反応物 | 2-Methylquinolin-4-ol | HCID 178428811 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 4-methoxyquinaldine-N-oxide | HCID 20401889 | — |
反応手順
31 g of 4-methoxyquinaldine (prepared from 4-hydroxyquinaldine by the method of M. Maurin, A. Ch. 4 [11] (1935), 301 and 335) are taken up in 80 ml of chloroform at room temperature, and 42 g of 85% strength m-chloroperbenzoic acid are added a little at a time, with stirring. The mixture is heated at 40° C. for 2 hours and is then cooled to 20° C. and brought to pH 6-7 with about 9 g of NaOH in 50 ml of H2O. The organic phase is separated off, dried with Na2SO4, filtered and concentrated. 34 g of crude product remain, and are recrystallized from toluene with addition of a small amount of solid KOH. 12 g of pure 4-methoxyquinaldine-N-oxide are obtained. Melting point 131°-132° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04510146 |
|---|
| 出典データセット | uspto-grants-1985_04 |
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| ORD ID | ord-053fda05c0284904ae7db291f2ab0146 |
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| 出典メモ | uspto-grants-1985_04 |
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