HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Barium bromate → 4-(3-Hydroxy-propyl)-6-(3-methylsulphamoyl-5-trifluoromethyl-phenyl)-pyrimidine-2-carbonitrile
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Barium bromate | HCID 61706 | — |
| Edukt | Cerous sulfate | HCID 159674 | — |
| Edukt | 4-(3-Benzyloxy-propyl)-6-(3-methylsulphamoyl-5-trifluoromethyl-phenyl)-pyrimidine-2-carbonitrile | HCID 69047005 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | 4-(3-Hydroxy-propyl)-6-(3-methylsulphamoyl-5-trifluoromethyl-phenyl)-pyrimidine-2-carbonitrile | HCID 57839126 | 27,2% |
Reaktionsschritte
To a solution of 4-(3-benzyloxy-propyl)-6-(3-methylsulphamoyl-5-trifluoromethyl-phenyl)-pyrimidine-2-carbonitrile (14.4 mg) in acetonitrile (700 μL) and water (300 μL) was added cerium sulphate (3 mg) and barium bromate (6 mg). The mixture was heated to reflux overnight then filtered through a sinter glass funnel, the residue washed with DCM (10 mL). The filtrate was washed with saturated sodium thiosulphate (10 mL) organics separated, dried over sodium sulphate, filtered, and solvent was removed under reduced pressure to yield crude product. Purification by preparative-H PLC afforded 4-(3-hydroxy-propyl)-6-(3-methylsulphamoyl-5-trifluoromethyl-phenyl)-pyrimidine-2-carbonitrile (3.2 mg).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07589095B2 |
| Quelldatensatz | uspto-grants-2009_09 |
| ORD ID | ord-5b4686ede87146bf8431d57f4bb1ca83 |
| Quellennotiz | uspto-grants-2009_09 |