تفاعل #66628

معادلة التفاعل

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

المردود 88.0%

ظروف التفاعل

المعالجة

1. 1
   أخرىSolvent was removed under reduced pressure and ice water
2. 2
   workup.ADDITIONwas added
3. 3
   استخلاصextracted with methylene chloride
4. 4
   غسيلThe organic phase was washed with brine
5. 5
   تجفيفdried over anhydrous sodium sulfate
6. 6
   أخرىAfter removal
7. 7
   أخرىof drying agent
8. 8
   تركيزthe organic solution was concentrated under reduced pressure

الإجراء التجريبي

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.

المصدر