Reaktion #66628

Reaktionsgleichung

2-amino-5-(2-isopropyl-4-methoxy-5-methyl-phenoxy)-3H-pyrimidin-4-one

phosphorus oxychloride

→

4-chloro-5-(2-isopropyl-4-methoxy-5-methyl-phenoxy)-pyrimidin-2-ylamine

Ausbeute 88.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeSolvent was removed under reduced pressure and ice water
2. 2
   workup.ADDITIONwas added
3. 3
   Extraktionextracted with methylene chloride
4. 4
   WaschenThe organic phase was washed with brine
5. 5
   Trocknendried over anhydrous sodium sulfate
6. 6
   SonstigeAfter removal
7. 7
   Sonstigeof drying agent
8. 8
   Einengenthe organic solution was concentrated under reduced pressure

Vorschrift

A mixture of 2-amino-5-(2-isopropyl-4-methoxy-5-methyl-phenoxy)-3H-pyrimidin-4-one in phosphorus oxychloride (5 ml) was heated at 110° C. for 40 minutes and stirred at room temperature over night. Solvent was removed under reduced pressure and ice water was added. The aqueous solution was basified with potassium carbonate to pH 9, and extracted with methylene chloride. The organic phase was washed with brine and dried over anhydrous sodium sulfate. After removal of drying agent, the organic solution was concentrated under reduced pressure to yield 4-chloro-5-(2-isopropyl-4-methoxy-5-methyl-phenoxy)-pyrimidin-2-ylamine as yellow solid (0.043 g, 88%). MS M+H=308.

Quelle