関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chlorotrimethylsilane | HCID 6397 | — |
| 反応物 | Benzenamine, N-sulfinyl- | HCID 70739 | — |
| 反応物 | 2,3-Difluoro-1,4-di(2-thienyl)-5,6-diamino-benzene | HCID 86670674 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 5,6-Difluoro-4,7-di(thiophen-2-yl)benzo[c][1,2,5]thiadiazole | HCID 66780891 | 99.1% |
反応手順
2,3-difluoro-1,4-di(2-thienyl)-5,6-diamino-benzene (1.2 g, 3.9 mmol) was added into a small flask and purged with Ar three times. Then, dry pyridine (24 ml), N-thionylaniline (1.08 g, 7.8 mmol) and chlorotrimethylsilane (0.76 g, 7.0 mmol) were added. The mixture was stirred at 80° C. for 16 h before poured into ice water. The yellow precipitate was then filtered and washed with a mixture of ethanol and water (1:1 v/v) to afford 5,6-difluoro-4,7-di(2-thienyl)-2,1,3-benzothiadiazole as a yellow solid (1.3 g, 98%). 1H and 19F NMR spectra were as expected.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08927684B2 |
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| 出典データセット | uspto-grants-2015_01 |
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| ORD ID | ord-25d68aae430148d3b11dbd5e66c1a1ae |
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| 出典メモ | uspto-grants-2015_01 |
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