HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
p-Chlorobenzenesulfonic acid → p-Toluenesulfonic acid monohydrate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | p-Chlorobenzenesulfonic acid | HCID 7400 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | Methylboronic Acid | HCID 139377 | — |
| Katalysator | palladium(II) acetate | HCID 167845 | — |
| Katalysator | Sodium 2'-(dicyclohexylphosphino)-2,6-dimethoxybiphenyl-3-sulfonate | HCID 23677046 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | p-Toluenesulfonic acid monohydrate | HCID 521998 | 217,6% |
Reaktionsschritte
The general procedure described in Example 3 was used with 4-chlorobenzenesulfonic acid (192 mg, 1.00 mmol), methylboronic acid (90 mg, 1.50 mmol), Pd(OAc)2 (2.2 mg, 0.010 mmol, 1 mol %), sodium 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl-3′-sulfonate (10.0 mg, 0.020 mmol, 2 mol %), K2CO3 (414 mg, 3.00 mmol), water (2.0 mL), 12 h, 100° C. The product was isolated as a white solid (207 mg, 99%). Mp=104° C. (lit.=106° C.). 1H NMR (400 MHz, d4-MeOH) δ: 7.71 (d, 2H, J=8.4 Hz), 7.24 (d, 2H, J=8.4 Hz), 5.08 (s, H2O), 2.37 (s, 3H)). 13C NMR (125 MHz, d4-MeOH) δ: 143.3, 142.0, 130.0, 127.1, 21.4.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07560596B2 |
| Quelldatensatz | uspto-grants-2009_07 |
| ORD ID | ord-0bf4d5c14d6f46f88cb67dcd1ee045b4 |
| Quellennotiz | uspto-grants-2009_07 |