Reacción #66628

Ecuación de reacción

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

Rendimiento 88.0%

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroSolvent was removed under reduced pressure and ice water
2. 2
   workup.ADDITIONwas added
3. 3
   Extracciónextracted with methylene chloride
4. 4
   LavadoThe organic phase was washed with brine
5. 5
   Secadodried over anhydrous sodium sulfate
6. 6
   OtroAfter removal
7. 7
   Otroof drying agent
8. 8
   Concentraciónthe organic solution was concentrated under reduced pressure

Procedimiento

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.

Fuente