関与物質
| 役割 | 名称 | HCID | 仕込み量 |
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| 反応物 | 4,7-Dibromo-2,1,3-benzothiadiazole | HCID 626361 | — |
| 反応物 | 2-(Tri-n-butylstannyl)thiophene | HCID 2779373 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4,7-Di(thiophen-2-yl)benzo(c)(1,2,5)thiadiazole | HCID 396294 | — |
反応手順
An analogous process is described by Kim et al. in “Journal of Material Chemistry” (2008), Vol. 18, pages 5223-5229, in which 4,7-di-2-thienyl-2,1,3-benzothia-diazole (DTB) can be prepared by reacting 4,7-dibromo -2,1,3-benzothiadiazole and tri-n-butyl(thien-2-yl)stannane, in the presence of tetrahydrofuran, at 66° C., for 3 hours. Bis(triphenylphosphine)palladium-(II)chloride [PdCl2(PPh3)2] is used as catalyst. Also in this case, at the end of the reaction, the solvent is removed by evaporation at reduced pressure and the residue obtained is purified by elution on a silica gel chromatographic column using a mixture of methylene chloride/hexane (1/1 vol/vol) as eluent, obtaining 4,7-di-2-thienyl-2,1,3-benzothiadiazole (DTB) with a yield equal to 88%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09353125B2 |
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| 出典データセット | uspto-grants-2016_05 |
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| ORD ID | ord-e98d1b91c944432081324df92623e01c |
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| 出典メモ | uspto-grants-2016_05 |
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