HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → 4-(7-Chloro-1,3-benzodioxol-5-yl)-2-pyrimidin-2-yl-5-(trifluoromethyl)pyrazol-3-amine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 2-Hydrazinylpyrimidine | HCID 346558 | — |
| Edukt | 3-Chloro-2-(7-chloro-1,3-benzodioxol-5-yl)-4,4,4-trifluoro-but-2-enenitrile | HCID 131733695 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | 4-(7-Chloro-1,3-benzodioxol-5-yl)-2-pyrimidin-2-yl-5-(trifluoromethyl)pyrazol-3-amine | HCID 90010064 | 44% |
Reaktionsschritte
3-chloro-2-(7-chloro-1,3-benzodioxol-5-yl)-4,4,4-trifluoro-but-2-enenitrile (20.2 g, 65.4 mmol) was dissolved in ethanol (200 mL) and treated with pyrimidin-2-yl-hydrazine (7.20 g, 65.4 mmol) and triethylamine (6.60 g, 65.4 mmol). The reaction mixture was heated to reflux for 10 h. The solvent was removed in vacuo, to the residue was added water, extracted with EtOAc, then the organic layer was combined, washed with water and brine, dried, filtered and concentrated to give crude product. The crude product was washed with DCM to give the title compound (11.0 g; 44%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09174967B2 |
| Quelldatensatz | uspto-grants-2015_11 |
| ORD ID | ord-ad6ad92f945645c5a0d9b2db56f7291b |
| Quellennotiz | uspto-grants-2015_11 |