HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → 2-Methyl-4-(6-phenylethynyl-pyridazin-3-ylamino)-butan-2-ol
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 3-Chloro-6-(phenylethynyl)pyridazine | HCID 12680260 | — |
| Edukt | 4-Amino-2-methylbutan-2-ol hydrochloride | HCID 42614560 | — |
| Lösungsmittel | Pyridine | HCID 1049 | — |
| Produkt | 2-Methyl-4-(6-phenylethynyl-pyridazin-3-ylamino)-butan-2-ol | HCID 57516775 | 27% |
Reaktionsschritte
A solution of 3-chloro-6-(phenylethynyl)pyridazine (CAS 77778-15-5) (125 mg, 0.582 mmol) and 4-amino-2-methylbutan-2-ol hydrochloride (244 mg, 1.75 mmol, 3 equiv.) and triethylamine (206 mg, 284 ml, 2.04 mmol, 2 equiv.) in 1.25 ml of pyridine was heated 20 hours at 85° C. The solvent was removed in vacuo. The residue was taken up in ethyl acetate/methanol, adsorbed onto 4 g of silica and purified on a 20 g flash chromatography column using a heptane/ethyl acetate 85:15 to 15:85 gradient to yield 44 mg (27% yield) of the title compound as a crystalline white solid, MS: m/e=282.2 (M+H+).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08513273B2 |
| Quelldatensatz | uspto-grants-2013_08 |
| ORD ID | ord-bb903643330642b69518ce094753364d |
| Quellennotiz | uspto-grants-2013_08 |