HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethyl Sulfate → 5-Bromo-3-methyl-2-(methylthio)pyrimidin-4(3H)-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethyl Sulfate | HCID 6497 | — |
| Edukt | Potassium Hydroxide | HCID 14797 | — |
| Edukt | 5-Bromo-2-(methylsulfanyl)pyrimidin-4(3H)-one | HCID 240565 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 5-Bromo-3-methyl-2-(methylthio)pyrimidin-4(3H)-one | HCID 3264666 | 94,5% |
Reaktionsschritte
To a mixture containing 0.70 g (5.5 mmol) of dimethyl sulfate and 0.25 g (4.5 mmol) of potassium hydroxide in 10 ml of tetrahydrofuran was added 0.5 g (2.25 mmol) of 5-Bromo-2-(methylthio)pyrimidin-4(3H)-one in portions over 15 min. After complete addition, the mixture was stirred overnight then diluted with ethyl acetate and washed with water. The organic phase was dried over magnesium sulfate. Filtration, removal of solvent and purification of the residue via Biotage chromatography eluting with 20% ethyl acetate/dichloromethane gave 0.5 g (94%) of product.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07897607B2 |
| Quelldatensatz | uspto-grants-2011_03 |
| ORD ID | ord-d4e65b5a47f349258865a7eb68080063 |
| Quellennotiz | uspto-grants-2011_03 |