HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Hydroxide → 6-[(Methyloxy)carbonyl]-2-pyridinecarboxylate potassium salt
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Hydroxide | HCID 14797 | — |
| Edukt | Dimethyl pyridine-2,6-carboxylate | HCID 79549 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 6-[(Methyloxy)carbonyl]-2-pyridinecarboxylate potassium salt | HCID 68632422 | 79% |
Reaktionsschritte
To a suspension of dimethyl 2,6-pyridinedicarboxylate (95.22 g, 488 mmol) in a 2 L round-bottom flask under nitrogen in methanol (1,200 mL; ˜12.5 volumes) was added powdered potassium hydroxide (27.4 g, 488 mmol). The mixture was stirred and after 3 min was almost all in solution. After 20 min lab HPLC showed a 33:62 ratio of starting material to product. Solvent was evaporated and the resulting solid was stirred well with 1000 mL ethyl acetate, then filtered under vacuum, then dried at 40° C. under high vacuum to give 84.5 g (79%) of a white solid that lab HPLC showed to be 98.2% pure (ret time 1.41 min). LC-MS m/z 182 (M+H)+, 0.57 min (ret time).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08084449B2 |
| Quelldatensatz | uspto-grants-2011_12 |
| ORD ID | ord-57ab9b8ca8b44f7bb1610342bd83a0a2 |
| Quellennotiz | uspto-grants-2011_12 |