関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-(Trifluoromethyl)aniline | HCID 7375 | — |
| 反応物 | 1-Chloro-6-methyl-5-nitroisoquinoline | HCID 22622221 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 6-Methyl-5-nitro-N-(3-(trifluoromethyl)phenyl)isoquinolin-l-amine | HCID 67339476 | 81.1% |
反応手順
1-Chloro-6-methyl-5-nitroisoquinoline (0.25 g, 1.1 mmol) and 3-(trifluoromethyl)benzenamine (0.17 mL, 1.3 mmol) were added to a microwave tube containing 3 mL of isopropanol. The tube was capped and heated at 180° C. for 1500 seconds. The volatiles were removed in vacuo. The residue was taken up in DCM and washed with saturated NaHCO3. The organic layer was dried with sodium sulfate and purified by column chromatography on silica gel using a gradient of 10 to 40% of ethyl acetate in hexanes to give the product as an orange solid (0.31 g, 79%). MS (M+H)+ 348.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07989461B2 |
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| 出典データセット | uspto-grants-2011_08 |
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| ORD ID | ord-de34fa00b71f4e169f579d51e8639b72 |
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| 出典メモ | uspto-grants-2011_08 |
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