Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 2-Chloro-3-fluoropyridin-4-amine | HCID 60150289 | — |
| Edukt | 2,6-Dichloro-4-iodobenzoyl chloride | HCID 86648958 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | HCID 86723309 | HCID 86723309 | 54% |
Reaktionsschritte
A mixture of 2-chloro-3-fluoropyridin-4-ylamine (1.73 g, 11.8 mmol), 2,6-dichloro-4-iodobenzoyl chloride (5.90 g, 17.65 mmol) and triethylamine (3.1 mL, 22.4 mmol) in dioxane (35 mL) was heated to 100° C. for 18 hours. The reaction mixture was partitioned between EtOAc and water. The organic layer washed with brine, dried over Na2SO4 and concentrated under reduced pressure. The resultant residue was triturated with diethyl ether and dried under reduced pressure to give the desired compound as a pink solid (2.83 g, 54% yield). 1H NMR (300 MHz, CDCl3): δ 8.49-8.43 (m, 1H), 8.22 (d, J=5.5 Hz, 1H), 7.82-7.73 (m, 2H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US08697708B2 |
|---|
| Quelldatensatz | uspto-grants-2014_04 |
|---|
| ORD ID | ord-5332521f85cb41eaaf7bc9d0707d3299 |
|---|
| Quellennotiz | uspto-grants-2014_04 |
|---|