HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Diisopropylethylamine → HCID 86711578, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | 4-Methylsulfonylbenzylamine hydrochloride | HCID 2729269 | — |
| Edukt | Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 2733084 | — |
| Edukt | 5-Bromo-1-isopropyl-6-methyl-4-oxo-1,4-dihydropyridine-3-carboxylic acid | HCID 86711577 | — |
| Lösungsmittel | Acetic Acid | HCID 176 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | HCID 86711578 | HCID 86711578 | — |
Reaktionsschritte
A solution of 5-bromo-1-isopropyl-6-methyl-4-oxo-1,4-dihydro-pyridine-3-carboxylic acid (preparation 3c, 0.50 g, 1.82 mmol), HBTU (0.77 g, 2.03 mmol), DIPEA (0.76 mL, 4.47 mmol) in DMF (2 mL) is stirred for 10 min. Then, 4-methylsulfonylbenzylamine hydrochloride (0.64 g, 2.89 mmol) is added and the reaction mixture is stirred for 72 h at room temperature. The reaction mixture is diluted with methanol, acidified with acetic acid and purified by preparative reversed-phase HPLC (XBridge, gradient of methanol in water, 0.1% TFA, 60° C.). Yield: 0.25 g (31% of theory); ESI mass spectrum: [M+H]+=441 (bromine isotope pattern); Retention time HPLC: 1.16 min (Z002_006).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09340507B2 |
| Quelldatensatz | uspto-grants-2016_05 |
| ORD ID | ord-9ee55156bda64e9b85d9075772213a1f |
| Quellennotiz | uspto-grants-2016_05 |