HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Benzyl Bromide → Methyl 4-benzyloxy-3-nitrobenzoate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Benzyl Bromide | HCID 7498 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | Benzoic acid, 4-hydroxy-3-nitro-, methyl ester | HCID 66835 | — |
| Lösungsmittel | Acetone | HCID 180 | — |
| Produkt | Methyl 4-benzyloxy-3-nitrobenzoate | HCID 289857 | — |
Reaktionsschritte
A solution of 4-hydroxy-3-nitro-benzoic acid methyl ester (30 g, 152 mmol) in acetone (1000 mL) was charged into a 2 L reactor and treated with K2CO3 (31.5 g, 228 mol) and benzyl bromide (52 g, 36.1 mL, 304 mmol). The mixture was mechanically stirred at heated at reflux for 16 hours under a light argon flux. After cooling to room temperature the solvent was evaporated. The residue was taken up in ethyl acetate/water and the two phases were separated. The aqueous phase was extracted three times with ethyl acetate (total solvent volume: 1.5 L, total water volume 1 L). The combined organic phases were dried over sodium sulfate and evaporated. 4-Benzyloxy-3-nitro-benzoic acid methyl ester thus obtained was used crude in the following reaction.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07696200B2 |
| Quelldatensatz | uspto-grants-2010_04 |
| ORD ID | ord-4c6f1f47224b4c09b3b659e71046e252 |
| Quellennotiz | uspto-grants-2010_04 |