Phosphorus oxychloride → 4-Chloro-6-methyl-2-(methylthio)pyrimidine
Reaktionsgleichung
O[C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([S:9][CH3:10])[N:3]=1.P(Cl)(Cl)([Cl:13])=O>>[Cl:13][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([S:9][CH3:10])[N:3]=1Komponenten
3
Versuchsvorschrift
4-Hydroxy-6-methyl-2-(methylthio)pyrimidine (9.20 g, 59 mmol) and phosphorous oxychloride (60 mL) were combined and refluxed for 3 hours. The reaction mixture was cooled to room temperature and poured onto crushed ice. The resultant aqueous mixture was extracted with ethyl acetate; and the organic layer washed with saturated aqueous sodium bicarbonate followed by a water wash, dried over magnesium sulfate, and dried in vacuo to give 4-chloro-6-methyl-2-(methylthio)pyrimidine (8.27 g, 80%), m.p. 37°-38° C.
Aufarbeitung
- temperaturerefluxed for 3 hours
- additionpoured
- customonto crushed ice
- extractionThe resultant aqueous mixture was extracted with ethyl acetate
- washand the organic layer washed with saturated aqueous sodium bicarbonate
- washwash
- dry with materialdried over magnesium sulfate
- customdried in vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-98a5dd7fdda34899b5a9b85033b0fa91
- Quelldatensatz
- uspto-grants-1999_01
- Patentnummer
- US05863924
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