HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Benyltrimethylammonium tetrachloroiodate → Ethyl 1-[6-(5-chloro-2-hydroxyphenyl)pyridin-2-yl]-5-(trifluoromethyl)-1H-pyrazole-4-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Benyltrimethylammonium tetrachloroiodate | HCID 57347110 | — |
| Edukt | Ethyl 1-[6-(2-hydroxylphenyl)pyridine-2-yl]-5-trifluoromethyl-1H-pyrazole-4-carboxylate | HCID 136298134 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | Ethyl 1-[6-(5-chloro-2-hydroxyphenyl)pyridin-2-yl]-5-(trifluoromethyl)-1H-pyrazole-4-carboxylate | HCID 136356800 | — |
Reaktionsschritte
To a solution of the title compound from Example 1 Step B (1.00 g, 2.65 mmol) in DCM (13 mL) was added benzyltrimethylammonium tetrachloroiodate (1.13 g, 2.70 mmol) and the resulting mixture was allowed to stir at ambient temperature. After 24 h, the mixture was concentrated in vacuo. Purification by chromatography on silica gel (0 to 18% EtOAc in hexanes, then 18 to 100% EtOAc in hexanes) provided the title compound: LCMS m/z 412.0 [M+H]+; 1H NMR (500 MHz, CDCl3) δ 11.98 (s, 1H), 8.18 (s, 1H), 8.10 (t, J=8.0 Hz, 1H), 8.00 (d, J=8.0 Hz, 1H), 7.78 (br s, 1H), 7.55 (d, J=8.0 Hz, 1H), 7.30 (dd, J=9.0, 2.0 Hz, 1H), 6.98 (d, J=9.0 Hz, 1H), 4.39 (q, J=7.0 Hz, 2H), 1.40 (t, J=7.0 Hz, 3H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08455638B2 |
| Quelldatensatz | uspto-grants-2013_06 |
| ORD ID | ord-104d531e77e54f7ebcf9e7c536977096 |
| Quellennotiz | uspto-grants-2013_06 |