HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
2,6-Dichlorobenzoic acid → Methyl 2,6-dichlorobenzoate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 2,6-Dichlorobenzoic acid | HCID 5758 | — |
| Edukt | Dimethyl Carbonate | HCID 12021 | — |
| Edukt | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | Methyl 2,6-dichlorobenzoate | HCID 599542 | 86% |
Reaktionsschritte
2,6-Dichlorobenzoic acid (5.00 g, 26.2 mmol) was diluted in dimethylcarbonate (44 mL, 530 mmol). 1,8-Diazabicyclo[5.4.0]undec-7-ene (DBU) (3.91 mL, 26.2 mmol) was added last. The reacted was refluxed for 2 days. Upon cooling, the solution was diluted with ethyl acetate and water. The aqueous layer was removed and the organic layer was washed with water, 2N HCl (2×'s), sat. NaHCO3 (2×'s), and twice with water. The organic layer was dried over sodium sulfate, filtered, and concentrated to yield 4.61 g (86%) of the desired compound as a clear oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07897607B2 |
| Quelldatensatz | uspto-grants-2011_03 |
| ORD ID | ord-e4b592d9e1174c3e8aa2d388ae8a49b5 |
| Quellennotiz | uspto-grants-2011_03 |