HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 2,3,4,5-tetrahydro-1H-1-benzazepine-2,5-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | Ethyl 4-(2-aminophenyl)-4-oxobutanoate | HCID 21283602 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 2,3,4,5-tetrahydro-1H-1-benzazepine-2,5-dione | HCID 369398 | 81% |
Reaktionsschritte
To a suspension of sodium hydride (10 mg, 0.43 mmol) in dry THF (1 mL) was added 4-(2-amino-phenyl)-4-oxo-butyric acid ethyl ester (80 mg, 0.36 mmol) under Argon at −40° C. The reaction mixture was then allowed to warm up to rt over 3 h, and then added to water (20 mL). The mixture was then extracted with DCM (3×15 mL) and the combined extracts were then dried (sodium sulfate), and evaporated to leave an off-white solid. Recrystallization from EtOAc afforded a white solid (51 mg, 81%), m/z 175 (M).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06686352B2 |
| Quelldatensatz | uspto-grants-2004_02 |
| ORD ID | ord-5ea0ac506de94e1ca90453849bbf16c6 |
| Quellennotiz | uspto-grants-2004_02 |