反应详情

温度

110 °C

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.

1. customSolvent was removed under reduced pressure and ice water
2. additionwas added
3. extractionextracted with methylene chloride
4. washThe organic phase was washed with brine
5. dry with materialdried over anhydrous sodium sulfate
6. customAfter removal
7. customof drying agent
8. concentrationthe organic solution was concentrated under reduced pressure