HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
HRID 2078166Erstellt: 25. Oktober 2026
Sodium Carbonate → 1,1-Dimethylethyl N-((7-phenyl-4-hydroxy-1,1-dimethyl-2-oxo-naphthalen-3-yl)carbonyl)glycinate
https://huagongshe.com/reaction/2078166
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | Phenylboronic Acid | HCID 66827 | — |
| Edukt | 1,1-Dimethylethyl N-((7-bromo-4-hydroxy-1,1-dimethyl-2-oxo-naphthalen-3-yl)carbonyl)glycinate | HCID 67099764 | — |
| Katalysator | HCID 178418397 | HCID 178418397 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | 1,1-Dimethylethyl N-((7-phenyl-4-hydroxy-1,1-dimethyl-2-oxo-naphthalen-3-yl)carbonyl)glycinate | HCID 67100007 | 69,2% |
Reaktionsschritte
1,1-Dimethylethyl N-((7-bromo-4-hydroxy-1,1-dimethyl-2-oxo-naphthalene-3-yl)carbonyl)glycinate (250 mg, 0.59 mmol, prepared in Example 53A-E), phenylboronic acid (108 mg, 0.9 mmol), tetrakis(triphenylphosphine)palladium (68 mg, 0.06 mmol), and 2M Na2CO3 (885 μL, 2 mmol) were mixed in dioxane (4 mL). The reaction vessel was placed under an argon atmosphere and stirred at 75° C. for 16 hours. The reaction mixture was cooled to room temperature and partitioned between EtOAc and water. The organic layer was separated, washed with brine, dried (MgSO4), and concentrated in vacuo to give the crude product. The crude product was purified by silica flash chromatography (0-100% DCM/hexane) to give the desired compound as a yellow solid (172 mg). MS (m/e)=366.2 (M+H-tBu)+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US07928139B2 |
|---|
| Quelldatensatz | uspto-grants-2011_04 |
|---|
| ORD ID | ord-6bc4cd13a3f64100ad339c6a3f46a761 |
|---|
| Quellennotiz | uspto-grants-2011_04 |
|---|