関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Tin tetrachloride | HCID 24287 | — |
| 反応物 | 6-Methyl-5-nitro-N-(3-(trifluoromethyl)phenyl)isoquinolin-l-amine | HCID 67339476 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 6-methyl-N1-(3-(trifluoromethyl)phenyl)isoquinoline-1,5-diamine | HCID 44478903 | 31% |
反応手順
6-Methyl-5-nitro-N-(3-(trifluoromethyl)phenyl)isoquinoline-1-amine (1.49 g, 4.29 mmol) obtained in Step (1) above was stirred in a solvent of ethanol (10 mL). The reaction solution was added with tin chloride (II) dihydrate (4.06 g, 21.46 mmol), and stirred for about 5 hours at 90° C. The reaction mixture was diluted with ethyl acetate, and washed with a saturated aqueous sodium bicarbonate solution and saline. The organic layer thus obtained was dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure to obtain the title compound (0.42 g, 31%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09388165B2 |
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| 出典データセット | uspto-grants-2016_07 |
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| ORD ID | ord-c58953cc22b8441388a9dd5c6cb91e2f |
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| 出典メモ | uspto-grants-2016_07 |
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