関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Nitrophenylboronic Acid | HCID 1677 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 2-Amino-5-bromo-3-iodobenzenesulphonic acid | HCID 18919385 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Amino-5-bromo-3'-nitro[1,1'-biphenyl]-3-sulphonic acid | HCID 11046967 | 80.4% |
反応手順
To a solution of 1.9 g (5 mmol) of 2-amino-5-bromo-3-iodobenzenesulphonic acid and 1.6 g (15 mmol) of sodium carbonate in 25 ml of dimethylformamide and 12.5 ml of water are added successively, under a nitrogen atmosphere, 0.231 g (0.2 mmol) of tetrakis(triphenylphosphine)palladium (0) and 1.42 g (8.5 mmol) of 3-nitrobenzeneboronic acid. The reaction medium is heated for 2 hours at 70° C. and is concentrated under reduced pressure. The residue thus obtained is purified by chromatography on an RP 18 reverse-phase column, eluting with an acetonitrile/water mixture (1:9). 1.5 g of compound are obtained in sodium sulphonate form.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05712393 |
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| 出典データセット | uspto-grants-1998_01 |
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| ORD ID | ord-862f5d7befe94e5a8b4a84ccb56443fe |
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| 出典メモ | uspto-grants-1998_01 |
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