참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Diisopropylamine | HCID 7912 | — |
| 반응물 | Trimethyltin chloride | HCID 14016 | — |
| 반응물 | 4,7-Di(thiophen-2-yl)benzo(c)(1,2,5)thiadiazole | HCID 396294 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Lithium diisopropylamide | HCID 2724682 | — |
| 생성물 | 2,1,3-Benzothiadiazole, 4,7-bis(5-(trimethylstannyl)-2-thienyl)- | HCID 58153009 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09296864B2 |
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| 출처 데이터셋 | uspto-grants-2016_03 |
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| ORD ID | ord-4d36d403e34f4f5eb6ff3d944dfca4b1 |
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| 출처 메모 | uspto-grants-2016_03 |
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