関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 1,3,4,5-Tetrahydro-2H-1-benzazepin-2-one | HCID 248580 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 7-nitro-2,3,4,5-tetrahydro-1H-1-benzazepin-2-one | HCID 356175 | — |
反応手順
2 g of 1,3,4,5-tetrahydro-2H-1-benzazepin-2-one are added to a solution of 25 ml of nitric acid at 70% in water and of 35 ml of sulfuric acid cooled to 0° C. The reaction medium is stirred for 15 minutes at 0° C. and then poured into water (250 ml) and extracted with ethyl acetate. The organic phase is washed with a saturated aqueous sodium bicarbonate solution and with water, dried over magnesium sulfate, filtered and concentrated under reduced pressure. The residue is taken up with diisopropyl ether and the insoluble material is filtered off and dried under vacuum, so as to give 1.04 g of 7-nitro-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one in the form of a beige solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09115140B2 |
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| 出典データセット | uspto-grants-2015_08 |
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| ORD ID | ord-a220b8ec54d947ea9832a6d3eb76f824 |
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| 出典メモ | uspto-grants-2015_08 |
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