関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Lawesson's reagent | HCID 87949 | — |
| 反応物 | 6-Bromo-8-chloro-3,4-dihydroquinolin-2(1H)-one | HCID 70979772 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 6-bromo-8-chloro-3,4-dihydroquinoline-2(1H)-thione | HCID 89961604 | — |
反応手順
To a stirred solution of 6-bromo-8-chloro-3,4-dihydroquinolin-2(1H)-one (80-1; 10 g, 0.038 mol) in toluene (130 mL) was added Lawesson's reagent (7.7 g, 0.019 mol). Reaction mass was refluxed at 100° C. for 3 h. The reaction mixture was concentrated and directly purified by silica gel column chromatography to obtain title compound. 1H NMR (400 MHz, DMSO-d6) δ: 11.25 (s, 1H), 7.61-7.60 (d, J=2.4 Hz, 1H), 7.48 (s, 1H), 2.96-2.93 (m, 2H), 2.85-2.81 (m, 2H). MS (M+2): 277.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09073929B2 |
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| 出典データセット | uspto-grants-2015_07 |
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| ORD ID | ord-82d59694bcf54d2a820b1e4ff8bb5270 |
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| 出典メモ | uspto-grants-2015_07 |
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