HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 6-Fluoropyridine-2-carbohydrazide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | 1,1-Dimethylethyl 2-[(6-fluoro-2-pyridinyl)carbonyl]hydrazinecarboxylate | HCID 66599038 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | 6-Fluoropyridine-2-carbohydrazide | HCID 345818 | 80,9% |
Reaktionsschritte
1,1-Dimethylethyl 2-[(6-fluoro-2-pyridinyl)carbonyl]hydrazinecarboxylate (510 mg, 2 mmol) was dissolved in 1,4-dioxane (5 mL) and treated with 4M HCl in 1,4 dioxane (5.00 mL, 20.00 mmol) at 0° C. The mixture was stirred to room temperature over 24 hr and was concentrated in vacuo, azeotroping with diethyl ether (3×50 ml) to afford a white solid. The solid was dissolved in methanol and loaded on to an SCX cartridge (Varian, 10 g), washing with methanol, and then eluting the product in free base form using 2M ammonia/methanol. The ammoniacal fractions were concentrated in vacuo to afford the product, 6-fluoro-2-pyridinecarbohydrazide (251 mg, 1.618 mmol).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08501946B2 |
| Quelldatensatz | uspto-grants-2013_08 |
| ORD ID | ord-209a4ad2708244e2b62bc0630c3eb4b8 |
| Quellennotiz | uspto-grants-2013_08 |