反応 #66628

反応方程式

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

収率 88.0%

反応条件

後処理

1. 1
   その他Solvent was removed under reduced pressure and ice water
2. 2
   workup.ADDITIONwas added
3. 3
   抽出extracted with methylene chloride
4. 4
   洗浄The organic phase was washed with brine
5. 5
   乾燥dried over anhydrous sodium sulfate
6. 6
   その他After removal
7. 7
   その他of drying agent
8. 8
   濃縮the organic solution was concentrated under reduced pressure

実験手順

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.

出典