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HRID 590527作成日:2026年10月25日
Lawesson's reagent → 2-bromo-2'-thioxo-6,7-dihydro-5H-spiro[benzo[b]thiophene-4,4'-imidazolidin]-5'-one
https://huagongshe.com/reaction/590527
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
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| 反応物 | Lawesson's reagent | HCID 87949 | — |
| 反応物 | 2-Bromo-6,7-dihydro-5H-spiro[benzo[b]thiophene-4,4'-imidazolidine]-2',5'-dione | HCID 90070540 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2-bromo-2'-thioxo-6,7-dihydro-5H-spiro[benzo[b]thiophene-4,4'-imidazolidin]-5'-one | HCID 90070542 | 97% |
反応手順
2-Bromo-6,7-dihydro-5H-spiro[benzo[b]thiophene-4,4′-imidazolidine]-2′,5′-dione (0.5 g, 1.67 mmol) and 2,4-bis(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane-2,4-disulfide (Lawesson's reagent) (0.371 g, 0.91 mmol) were suspended in 1,4-dioxane (5 mL). The mixture was heated by microwave irradiation at 110° C. for 2×30 min. The solution was concentrated in vacuo and the crude residue purified on silica gel using ethyl acetate in 40-60 petroleum ether (1:1) to afford the title compound as a colourless solid (0.28 g, 53%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09233982B2 |
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| 出典データセット | uspto-grants-2016_01 |
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| ORD ID | ord-840c475f24e146dc8c14d46e1b003c63 |
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| 出典メモ | uspto-grants-2016_01 |
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