HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Diisopropylethylamine → US9296748, III-1
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | N(1)-methyl-2-pyridone-5-carboxylic acid | HCID 592704 | — |
| Edukt | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| Edukt | N2-benzyl-6-(4-methylpiperazin-1-yl)pyridine-2,3-diamine | HCID 117892005 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | US9296748, III-1 | HCID 117889570 | — |
Reaktionsschritte
DIPEA (51 mg; 0.392 mmol) is added to a suspension of 1-methyl-6-oxo-1,6-dihydro-pyridine-3-carboxylic acid D-7 (20 mg; 0.131 mmol) and HATU (70 mg; 0.183 mg) in DMF. The mixture is stirred at RT for 5 min. N2-Benzyl-6-(4-methyl-piperazin-1-yl)-pyridine-2,3-diamine E-3.1 is then added and the reaction mixture stirred at RT for 1 h. The reaction mixture is extracted with DCM and NaHCO3 solution. The organic layer is dried over Na2SO4 and concentrated in vacuum. To the formed amide is added 1 ml glacial acetic acid, the reaction is stirred at 120° C. for 2 days. The crude reaction mixture is purified by using reversed phase chromatography (Method: prep. HPLC1).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09296748B2 |
| Quelldatensatz | uspto-grants-2016_03 |
| ORD ID | ord-3db050a642db4dc68a791dd85db22df9 |
| Quellennotiz | uspto-grants-2016_03 |