HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Tributylphosphine → 4'-({4-butyl-1-[(1,5-dimethyl-1H-pyrazol-3-yl)methyl]-2-methyl-6-oxo-1,6-dihydropyrimidin-5-yl}methyl)biphenyl-2-carbonitrile
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Tributylphosphine | HCID 13831 | — |
| Edukt | 1,1'-(Azodicarbonyl)dipiperidine | HCID 73042 | — |
| Edukt | (1,5-Dimethyl-1H-Pyrazol-3-Yl)Methanol | HCID 2776366 | — |
| Edukt | 4'-[(4-Butyl-2-methyl-6-oxo-1,6-dihydropyrimidin-5-yl)methyl]biphenyl-2-carbonitrile | HCID 135401222 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 4'-({4-butyl-1-[(1,5-dimethyl-1H-pyrazol-3-yl)methyl]-2-methyl-6-oxo-1,6-dihydropyrimidin-5-yl}methyl)biphenyl-2-carbonitrile | HCID 57460236 | 61,4% |
Reaktionsschritte
A mixture of 4′-[(4-butyl-2-methyl-6-oxo-1,6-dihydropyrimidin-5-yl)methyl]biphenyl-2-carbonitrile (1 g), 1,1′-(azodicarbonyl)dipiperidine (1.41 g), tributylphosphine (1.56 mL), (1,5-dimethyl-1H-pyrazol-3-yl)methanol (0.53 g) and tetrahydrofuran (50 mL) was stirred at room temperature for 4 hr. The reaction mixture was diluted with ethyl acetate, washed with water and then with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography to give the title compound as a colorless solid (0.80 g, 61%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07998968B2 |
| Quelldatensatz | uspto-grants-2011_08 |
| ORD ID | ord-4a86d5581eca44a5a10fe6444f9f360a |
| Quellennotiz | uspto-grants-2011_08 |