HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium hydride → HCID 178422572, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 2,6-Dichloropurine | HCID 5324412 | — |
| Edukt | 4-Cyclopropyl-2,6-dimethylphenol | HCID 57693555 | — |
| Lösungsmittel | 1-Methyl-2(1H)-pyridinone | HCID 12755 | — |
| Produkt | HCID 178422572 | HCID 178422572 | 67,1% |
Reaktionsschritte
To a solution of 4-cyclopropyl-2,6-dimethylphenol (263 mg, 1.62 mmol) in 1-methyl-2-pyridone (3 mL) at 0° C. was added NaH (65 mg, 1.62 mmol). The reaction mixture was stirred at room temperature for 30 min and a solution of 2,6-dichloropurine (102 mg, 0.54 mmol) in 1-methyl-2-pyridone (2 mL) was added to the mixture. The mixture was heated at 100° C. for 16 h and then cooled to room temperature. The reaction was poured into ice water and extracted with CHCl3 (3×20 mL). The combined organic solution was washed with H2O (20 mL) and brine (20 mL), dried with Na2SO4, and concentrated to dryness. Silica gel chromatography (MeOH:CHCl3=5:95) yielded 114 mg (67%) of 2-chloro-6-(4-cyclopropyl-2,6-dimethylphenoxy)-9H-purine.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08227601B2 |
| Quelldatensatz | uspto-grants-2012_07 |
| ORD ID | ord-a83f4a1a843a4498948c1c4c931e0e42 |
| Quellennotiz | uspto-grants-2012_07 |