HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Trifluoroacetic acid → HCID 67249920, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Trifluoroacetic acid | HCID 6422 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | (R)-tert-butyl 1-(4-(2-bromo-5-fluorobenzyl)-6-methyl-5-oxo-4,5-dihydro-1,2,4-triazin-3-yl)piperidin-3-ylcarbamate | HCID 58328539 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | HCID 67249920 | HCID 67249920 | — |
Reaktionsschritte
To a solution of (R)-tert-butyl 1-(4-(2-bromo-5-fluorobenzyl)-6-methyl-5-oxo-4,5-dihydro-1,2,4-triazin-3-yl)piperidin-3-ylcarbamate (18, 30 mg) in dichloromethane (1 mL) was added TFA (0.5 mL), and the mixture was stirred at RT for 3 h. The mixture was carefully neutralized with NaHCO3 (aq, saturated), and extracted with CH2Cl2 (10 mL×3). The combined extracts were dried over Na2SO4 and concentrated to give the crude product. This was purified by column chromatography on silica gel, and eluted with 92:6:2 dichloromethane-methanol-ammonia to provide (R)-3-(3-aminopiperidin-1-yl)-4-(3-fluorobenzyl)-6-methyl-1,2,4-triazin-5(4H)-one (19). MS: m/z, 396 (100%, M+1), 398 (100%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08648073B2 |
| Quelldatensatz | uspto-grants-2014_02 |
| ORD ID | ord-005f7eeefaa94590b480d68baa0784dc |
| Quellennotiz | uspto-grants-2014_02 |