関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethynylpyridine | HCID 137268 | — |
| 反応物 | 2-(3,4-Dimethoxybenzenesulphonyl)-4-bromoisoindoline | HCID 19689661 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 触媒 | Dichlorobis(triphenylphosphine)palladium | HCID 6102075 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-(3,4-Dimethoxybenzenesulphonyl)-4-(2-pyrid-2-ylethynyl)isoindoline | HCID 19689640 | 12.5% |
反応手順
2-(3,4-Dimethoxybenzenesulphonyl)-4-bromoisoindoline (0.19 g), triethylamine (0.10 ml), 2-ethynylpyridine(0.06 g) and bis (triphenylphosphine)palladium(II)chloride (10%) in anhydrous N,N-dimethylformamide(2 ml) were stirred together under an inert atmosphere and heated to 90° C. After 20 hours further 2-ethynylpyridine(0.12 g) and palladium catalyst (20%) were added and heating continued for 3 days. The reaction mixture at room temperature was diluted with ethyl acetate, filtered through a pad of silica and the filtrate evaporated in vacuo to yield a yellow residue. Purification by column chromatography, eluting with a 20-100% ethyl acetate in hexane gradient afforded the title compound (25 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05728712 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-1fbe8bec2d7a4b37b8e811f839c2b36c |
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| 出典メモ | uspto-grants-1998_03 |
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