HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hexane → 4,5-Dichloro-2-(2-phenyl-propionylamino)-benzoic acid methyl ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hexane | HCID 8058 | — |
| Edukt | 2-Phenylpropionic acid | HCID 10296 | — |
| Edukt | Thionyl Chloride | HCID 24386 | — |
| Edukt | Methyl 2-amino-4,5-dichlorobenzoate | HCID 11694243 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 4,5-Dichloro-2-(2-phenyl-propionylamino)-benzoic acid methyl ester | HCID 68815872 | 95% |
Reaktionsschritte
The objective compound was prepared by the same procedure for the intermediate 1, using a 2-phenyl-propionic acid (2.00 g, 13.3 mmol), SOCl2 (2.28 mL, 40.0 mmol), and 2-amino-4,5-dichloro-benzoic acid methyl ester (1.95 g, 8.88 mmol). After normal workup, the pure objective compound (2.97 g, 95%) was obtained as pale yellow solid by a flash column chromatography (n-hexane:EtOAc=20:1): 1H NMR (200 MHz, CDCl3) δ 1.59 (d, J=7.1 Hz, 3H, CH3), 3.70-3.89 (m, 4H, CO2CH3& CH), 7.28-7.42 (m, 5H, ArH), 8.03 (s, 1H, ArH), 8.99 (s, 1H, ArH), 11.00 (br s, 1H, NH).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07592457B2 |
| Quelldatensatz | uspto-grants-2009_09 |
| ORD ID | ord-0333392e559d465d84809f496bdfa882 |
| Quellennotiz | uspto-grants-2009_09 |