HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Acetic Anhydride → Ethyl 1,2-dimethyl-1,3-benzodiazole-5-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Acetic Anhydride | HCID 7918 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | Ethyl 3-amino-4-(methylamino)benzoate | HCID 2824047 | — |
| Produkt | Ethyl 1,2-dimethyl-1,3-benzodiazole-5-carboxylate | HCID 12493640 | — |
Reaktionsschritte
Ethyl 3-amino-4-methylaminobenzoate (1.00 g, 5.15 mmol) prepared in the Step 1-1-3 was dissolved in acetic anhydride (4 ml), and the mixture was heated under reflux for 19 hours. After being allowed to cool, the mixture was neutralized with a saturated sodium bicarbonate solution and subjected to extraction with ethyl acetate. The extract was dried over anhydrous magnesium sulfate and then concentrated. The concentrate was purified by silica gel column chromatography (chloroform:methanol=10:1) to give the title compound (1.15 g, quantitative) as a light-brown oily substance.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09200008B2 |
| Quelldatensatz | uspto-grants-2015_12 |
| ORD ID | ord-eb77b943f797455bb90af7eae8fb00eb |
| Quellennotiz | uspto-grants-2015_12 |