関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | N,N-Dimethylethylenediamine | HCID 66053 | — |
| 反応物 | 2-Bromobenzaldehyde | HCID 81129 | — |
| 反応物 | Sodium 4-bromobenzene-1-sulfinate | HCID 23670685 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | HCID 21099420 | HCID 21099420 | 55% |
反応手順
2-Bromobenzaldehyde (1.55 g, 8.4 mmol), sodium 4-bromophenylsulfinate (2.79 g, 10 mmol) and copper(I) trifluoromethanesulfonate benzene complex (500 mg, 1 mmol) were combined in dimethylsulfoxide (10 mL) under nitrogen and degassed. The suspension was heated to 110° C. and N,N-dimethylethylenediamine (176 mg, 2 mmol) was added. The reaction was heated until the colour became clear and pale yellow, then cooled and poured into water. The products were extracted into ethyl acetate. The organic layer was washed with water:brine (1:1, ×5), dried over MgSO4 and evaporated in vacuo. The residue was triturated with isohexane to give 2-[(4-bromophenyl)sulfonyl]benzaldehyde (1.5 g, 55%). δH (400 MHz, CDCl3): 10.76 (1H, s), 8.14-8.12 (1H, m), 7.98-7.96 (1H, m), 7.76-7.68 (4H, m), 7.64-7.62 (2H, m).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07468393B2 |
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| 出典データセット | uspto-grants-2008_12 |
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| ORD ID | ord-e1dcaa7d07224a34bfef95711daf4f48 |
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| 出典メモ | uspto-grants-2008_12 |
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