HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → HCID 178501494, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| Edukt | Methyl valinate hydrochloride | HCID 111190 | — |
| Edukt | 6-Bromopyridine-2-carbaldehyde | HCID 2757009 | — |
| Produkt | HCID 178501494 | HCID 178501494 | — |
Reaktionsschritte
Anhydrous magnesium sulfate (5.4 g), 6-bromopyridine-2-carboxaldehyde (5.0 g, 26.9 mmol) and triethylamine (3.75 mL, 26.9 mmol) were each added sequentially in one portion to a cooled (0° C.) solution of (L)-valine methyl ester hydrochloride (4.51 g, 26.9 mmol) and the reaction mixture was allowed to warm slowly to room temperature overnight under a nitrogen atmosphere. The mixture was then filtered and the filter cake washed with diethyl ether (100 mL) before evaporating the filtrate in vacuo. The residue was purified by column chromatography using 5:1 hexane/ethyl acetate as eluent to yield A469.1 (7.1 g, 88%). HPLC YMC S-5 4.6×33 mm (2 min grad): retention time 0.86 min, M+H+=202.08
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07737279B2 |
| Quelldatensatz | uspto-grants-2010_06 |
| ORD ID | ord-579292326f8242fabf3213cdbc438ee7 |
| Quellennotiz | uspto-grants-2010_06 |