HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Stannous chloride dihydrate → 2-Amino-4-(benzyloxy)-5-methoxybenzoic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Stannous chloride dihydrate | HCID 61436 | — |
| Edukt | 4-(Benzyloxy)-5-methoxy-2-nitrobenzoic acid | HCID 10859633 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 2-Amino-4-(benzyloxy)-5-methoxybenzoic acid | HCID 10967675 | — |
Reaktionsschritte
A solution of 4-benzyloxy-5-methoxy 2-nitrobenzoic acid (18.18 g, 60 mmol)(D. E. Thurston et al., Synthesis (1990), 81) and SnCl2.2H2O (137 g, 0.6 mol) (Showa Chemical Company, Japan) in MeOH (800 mL) was stirred at 70° C. for 5 h. The mixture was concentrated under vacuum to a thick syrup. Ethyl acetate (300 mL) was then added. The organic phase was washed with water until it turned to a clear solution, then washed with brine, and dried over MgSO4. After removal of solvent, the crude was recrystallized from ethyl acetate to obtain the title compound in the form of a yellow solid with a yield of 15.1 g (92%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06660856B2 |
| Quelldatensatz | uspto-grants-2003_12 |
| ORD ID | ord-87f565170a074cf9858bf3687fb98661 |
| Quellennotiz | uspto-grants-2003_12 |