참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Phenylboronic Acid | HCID 66827 | — |
| 반응물 | 2-Amino-5-bromo-3-iodobenzenesulphonic acid | HCID 18919385 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 생성물 | 2-Amino-5-bromo[1,1'-biphenyl]-3-sulphonic acid | HCID 18931667 | — |
반응 단계
To a mixture of 37.8 g (100 mmol) of 2-amino-5-bromo-3-iodobenzenesulphonic acid and 32 g (300 mmol) of sodium carbonate in 300 ml of 1,2-dimethoxyethane and 150 ml of water are successively added, under a nitrogen atmosphere, 5.8 g (5 mmol) of tetrakis(triphenylphosphine)palladium (0) and 19.5 g (160 mmol) of benzeneboronic acid. The mixture is heated at the reflux temperature for 4 hours and the reaction medium is then concentrated under reduced pressure. The residue thus obtained is then dissolved in a mixture containing 300 ml of methanol, 300 ml of 0.1N hydrochloric acid and 16 ml of 95% sulphuric acid. The mixture is concentrated to 100 ml under reduced pressure, cooled to 0° C. and filtered. The residue is purified by chromatography on an RP 18 reverse-phase column, eluting with an acetonitrile:water mixture (2:8).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05712393 |
|---|
| 출처 데이터셋 | uspto-grants-1998_01 |
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| ORD ID | ord-9d0f647a178945ec88aa837ce90d1f64 |
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| 출처 메모 | uspto-grants-1998_01 |
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