関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzylamine | HCID 7504 | — |
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | 2-Benzothiazol-2-yl-3,3-bis-methylsulfanylacrylonitrile | HCID 2807727 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 178509283 | HCID 178509283 | 53% |
反応手順
A solution of 2-benzothiazol-2-yl-3,3-bismethylsulfanylacrylonitrile (200 mg, 0.73 mmol) and benzylamine (160 mg, 1.5 mmol) in 50 mL of ethanol was heated to reflux for 90 minutes. Hydrazine hydrate (35 μL, 1.0 mmol) was then added to the reaction mixture. The solution was heated to reflux until the reaction was complete as determined by TLC analysis. The reaction solution was allowed to cool to room temperature and the title compound (124 mg) was isolated by filtration, washed with ethanol and dried under high vacuum. MS (m/z, ES+): 322 (M+1, 100%); 1H NMR (300 MHz, ppm, DMSO-d6): δμ11.32 (br s, 1/3H), 10.89 (s, br., 2/3H), 7.98 (d, 3J=7.7 Hz, 1H), 7.82 (d, 3J=8.0 Hz, 1H), 7.41-7.28 (m, 6H), 7.22 (m, 1H), 6.15 (br s, 9/10H), 4.95 (br s, 1/10H), 4.48 (d, 3J=4.7 Hz, 1H). Yield=53%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09434720B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-b9c15dfee0ca4b36b171547a69834048 |
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| 出典メモ | uspto-grants-2016_09 |
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