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
According to what is described by Kitamura et al. in “Chemistry of Material” (1996), Vol. 8, pages 570-578, for example, 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, in a quantity equal to 2 moles per 100 moles of 4,7-dibromo-2,1,3-benzothiadiazole. 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 82%.
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-6e424d0149d0477ca912322c0c27592f |
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| 出典メモ | uspto-grants-2016_05 |
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