HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 4,6-Bis(4-fluorophenyl)-5-(4-pyridyl)-1H-pyrazolo[3,4-b]pyridine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Pyrazol-3-ylamine | HCID 74561 | — |
| Edukt | 1-(4-Fluorophenyl)-2-(pyridin-4-yl)ethan-1-one | HCID 10330881 | — |
| Lösungsmittel | Chloroform | HCID 6212 | — |
| Lösungsmittel | 2-Methoxyethanol | HCID 8019 | — |
| Produkt | 4,6-Bis(4-fluorophenyl)-5-(4-pyridyl)-1H-pyrazolo[3,4-b]pyridine | HCID 11961374 | 47,2% |
Reaktionsschritte
In a volumetric flask, 1-(4-fluorophenyl)-2-(4-pyridyl)ethanone (23.56 g, 109.4 mmol, obtained in reference example 1) and 2-methoxyethanol (150 mL) were introduced. A solution of 3-amino-2H-pyrazole (10.00 g, 120.3 mmol) in 2-methoxyethanol (170 mL) and 37% HCl (3.23 g, 32.8 mmol) were added under argon atmosphere. This was heated to reflux for 3 days. It was allowed to cool and concentrated. The solid obtained was dissolved in CHCl3 (400 mL) and MeOH (50 mL) and washed with 0.1 N HCl (300 mL) and 1 N NaOH (300 mL). The organic phase was dried over Na2SO4 and concentrated to dryness, to afford 9.93 g of the desired product in solid cream form (yield: 47%)
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08536194B2 |
| Quelldatensatz | uspto-grants-2013_09 |
| ORD ID | ord-ad1fdfc90d014991bffdfe53fb8e0465 |
| Quellennotiz | uspto-grants-2013_09 |