Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | 3-Nitrophenylboronic Acid | HCID 1677 | — |
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | 2-Amino-5-bromo-3-iodobenzenesulphonic acid | HCID 18919385 | — |
| Katalysator | HCID 178418397 | HCID 178418397 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | HCID 11046967 | HCID 11046967 | 80,4% |
Reaktionsschritte
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.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US05712393 |
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| Quelldatensatz | uspto-grants-1998_01 |
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| ORD ID | ord-862f5d7befe94e5a8b4a84ccb56443fe |
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| Quellennotiz | uspto-grants-1998_01 |
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