HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Hydroxide → 5-Cyclopropylamino-6-cyclopropylmethoxy-pyridine-2-carboxylic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | 5-(Cyclopropylamino)-6-(cyclopropylmethoxy)-pyridine-2-carboxylic acid methyl ester | HCID 71087752 | — |
| Lösungsmittel | Ethylacetate methanol | HCID 21584119 | — |
| Produkt | 5-Cyclopropylamino-6-cyclopropylmethoxy-pyridine-2-carboxylic acid | HCID 71087191 | 92,1% |
Reaktionsschritte
A solution of 5-(cyclopropylamino)-6-(cyclopropylmethoxy)-pyridine-2-carboxylic acid methyl ester (400 mg, 1.53 mmol), sodium hydroxide (244 mg, 6.1 mmol) in THF/H2O 1/1 (10 mL) was stirred for 1 h at room temperature. The reaction mixture was concentrated under reduced pressure. Water was added and the pH was adjusted to 2 by addition of 1 N HCl. Extraction with ethyl acetate (30 mL) was followed by washing with brine (6×30 mL). The organic layer was dried over sodium sulfate and concentrated in vacuo. The residue was purified by column chromatography (silica gel, 50 g, 50% ethyl acetate in petroleum ether) to yield the title compound (350 mg, 92%) as yellow solid; MS (EI): m/e=249.3 [M+H]+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09290451B2 |
| Quelldatensatz | uspto-grants-2016_03 |
| ORD ID | ord-0667f5598a784fb8bee7a691aef4de30 |
| Quellennotiz | uspto-grants-2016_03 |