반응 #66628

반응 방정식

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

수율 88.0%

반응 조건

후처리

1. 1
   기타Solvent was removed under reduced pressure and ice water
2. 2
   workup.ADDITIONwas added
3. 3
   추출extracted with methylene chloride
4. 4
   세척The organic phase was washed with brine
5. 5
   건조dried over anhydrous sodium sulfate
6. 6
   기타After removal
7. 7
   기타of drying agent
8. 8
   농축the organic solution was concentrated under reduced pressure

실험 절차

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.

출처