Реакция #66628

Уравнение реакции

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

Выход 88.0%

Условия реакции

Обработка

1. 1
   ДругоеSolvent was removed under reduced pressure and ice water
2. 2
   workup.ADDITIONwas added
3. 3
   Экстракцияextracted with methylene chloride
4. 4
   ПромывкаThe organic phase was washed with brine
5. 5
   Сушкаdried over anhydrous sodium sulfate
6. 6
   ДругоеAfter removal
7. 7
   Другоеof drying agent
8. 8
   Концентрированиеthe organic solution was concentrated under reduced pressure

Методика

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.

Источник