Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Tripropylamine | HCID 7616 | — |
| Edukt | Phosphorus oxychloride | HCID 24813 | — |
| Edukt | 6-tert-Butyl-2-(2-trifluoromethyl-phenyl)-3H-pyrimidin-4-one | HCID 136157190 | — |
| Produkt | HCID 178441234 | HCID 178441234 | 66% |
Reaktionsschritte
A solution of 6-tert-butyl-2-(2-trifluoromethyl-phenyl)-3H-pyrimidin-4-one (0.47 g, 1.59 mmol) in phosphorous oxychloride (1.65 mL, 15.9 mmol) was treated with tri-n-propylamine (0.61 mL, 3.17 mmol) and heated at 110-120° C. for 1 hour. The solvent was removed by evaporation then azeotroped three times with toluene. The residue was taken up in ethyl acetate, washed sequentially with 1 N sodium hydroxide, water and brine, then dried over sodium sulfate and concentrated. Purification by flash chromatography [SiO2, ethyl acetate:hexanes (1:9)] provided the title compound (0.33 g, 66% yield) as a yellow oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07872129B2 |
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| Quelldatensatz | uspto-grants-2011_01 |
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| ORD ID | ord-135cbbe0ce6c44c7ae3e2d00695678d9 |
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| Quellennotiz | uspto-grants-2011_01 |
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