関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylamine | HCID 7912 | — |
| 反応物 | Trimethyltin chloride | HCID 14016 | — |
| 反応物 | 4,7-Di(thiophen-2-yl)benzo(c)(1,2,5)thiadiazole | HCID 396294 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Lithium diisopropylamide | HCID 2724682 | — |
| 生成物 | 2,1,3-Benzothiadiazole, 4,7-bis(5-(trimethylstannyl)-2-thienyl)- | HCID 58153009 | — |
反応手順
Compound (1) was dissolved in anhydrous THF (20 ml) in a nitrogen-filled flask. The solution was cooled down to −78° C. LDA was prepared from the reaction of diisopropylamine (0.5 g, 5.1 mmol, 3 eq.) and n-BuLi (3.12 ml, 5.1 mmol, 3 eq.) (1.6 M hexane solution) in anhydrous THF (2 ml), which was added to the above solution dropwise. After stirring for 1 h, trimethylstannyl chloride (3.8 ml, 3.8 mmol, 2.3 eq.) (1 M THF solution) was added and reacted for 1 h. The reaction was quenched by addition of water and the organic layer was extracted with ether, washed with water and dried over anhydrous magnesium sulfate. After the solvent was removed under reduced pressure, the residue was purified by recrystallization from ethanol, giving the title compound as a needle-shaped purple crystal.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09296864B2 |
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| 出典データセット | uspto-grants-2016_03 |
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| ORD ID | ord-4d36d403e34f4f5eb6ff3d944dfca4b1 |
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| 出典メモ | uspto-grants-2016_03 |
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