HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dibenz(b,f)azepine → (Z)-methyl 4-((5H-dibenzo[b,f]azepin-5-yl)methyl)benzoate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dibenz(b,f)azepine | HCID 9212 | — |
| Edukt | Dibutyltin dichloride | HCID 12688 | — |
| Edukt | Phenylsilane | HCID 12752 | — |
| Edukt | Methyl 4-Formylbenzoate | HCID 15294 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | (Z)-methyl 4-((5H-dibenzo[b,f]azepin-5-yl)methyl)benzoate | HCID 59783517 | 83% |
Reaktionsschritte
(Z)-5H-Dibenzo[b,f]azepine (100 mg, 0.52 mmol), dibutyltin dichloride (54 mg, 0.16 mmol) and methyl 4-formylbenzoate (260 mg, 1.60 mmol) were stirred in THF (2 mL) for 30 minutes. Phenylsilane was added and the reaction mixture was stirred for 3 days. The solvent was evaporated and the residue was purified by flash chromatography (0% to 40% EtOAc in hexanes). The fractions containing some product were washed with Na2S2O4. The layers were split and the organic layer was evaporated to afford title compound 350 (147 mg, 83%) as a yellow solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09193749B2 |
| Quelldatensatz | uspto-grants-2015_11 |
| ORD ID | ord-7abb1a6f4fef4ff6bddca28cd544f8f0 |
| Quellennotiz | uspto-grants-2015_11 |