HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 4,6-Dichloronicotinic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Methanol | HCID 887 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | Methyl4,6-dichloronicotinate | HCID 2764083 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 4,6-Dichloronicotinic acid | HCID 817158 | 69% |
Reaktionsschritte
To a solution of methyl 4,6-dichloronicotinate in a mixture of THF (400 ml), MeOH (100 ml) and H2O (100 ml) was added a solution of NaOH (10 g) in 40 ml H2O. The mixture was stirred for 40 min, at room temp. Then, the solvents were reduced and it was acidified with conc. HCl to a pH of about 2. It was extracted using a mixture of Et2O/EtOAc and the organic layer was dried with Na2SO4. The solvents were removed and the residue dried in vacuo to obtain the title compound as a white solid (12.3 g, 69%). Rf (CHCl3/MeOH 10:1)=0.85. 1H-NMR (300 MHz, DMSO-D6): δ=8.80 (s, 1H), 7.90 (s, 1H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08063049B2 |
| Quelldatensatz | uspto-grants-2011_11 |
| ORD ID | ord-02eb429e518f40d4baca2a1280997167 |
| Quellennotiz | uspto-grants-2011_11 |