HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethyl acetylsuccinate → HCID 178499491, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethyl acetylsuccinate | HCID 112039 | — |
| Edukt | 3-(3-chlorophenyl)-1H-pyrazol-5-amine | HCID 178507281 | — |
| Katalysator | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Lösungsmittel | O-Xylene | HCID 7237 | — |
| Produkt | HCID 178499491 | HCID 178499491 | 99% |
Reaktionsschritte
To a solution of 3-(3-chlorophenyl)-1H-pyrazol-5-amine (23 g, 119 mmol), dimethyl 2-acetylsuccinate (22.35 g, 119 mmol) in o-Xylene (200 mL) was added p-toluenesulfonic acid monohydrate (100 mg, 0.526 mmol). The reaction mixture was heated at reflux under a Dean-Stark trap for 2 h. The solid was filtered and washed with hexanes to afford (39 g, 99%) of the title compound. 1H NMR (500 MHz, METHANOL-d4) δ 8.14-7.95 (m, 1H), 7.93-7.79 (m, 1H), 7.51-7.27 (m, 2H), 6.62-6.35 (m, 1H), 3.72 (s, 3H), 3.67 (s, 2H), 2.39 (s, 3H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08633200B2 |
| Quelldatensatz | uspto-grants-2014_01 |
| ORD ID | ord-c028003bb1d5422ca0439088bbb4d68e |
| Quellennotiz | uspto-grants-2014_01 |