تفاعل #1103642

معادلة التفاعل

2,5-Dimethyl-4H-pyrazolo[1,5-a]pyrimidin-7-one

phosphorus oxychloride

→

title compound

المردود 77.0%

7-Chloro-2,5-dimethyl-pyrazolo[1,5-a]pyrimidine

المردود 77.0%

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةat reflux
2. 2
   أخرىAfter 3 hours the dark purple reaction
3. 3
   درجة الحرارةwas cooled
4. 4
   استخلاصextracted from ice water with ethyl acetate
5. 5
   غسيلThe combined organic layers were washed with water and saturated aqueous sodium bicarbonate
6. 6
   تجفيفdried (Na2SO4)
7. 7
   تركيزconcentrated under reduced pressure

الإجراء التجريبي

2,5-Dimethyl-4H-pyrazolo[1,5-a]pyrimidin-7-one (3.5 g, 21 mmol) in phosphorus oxychloride (20 mL) was stirred at reflux. After 3 hours the dark purple reaction was cooled and then extracted from ice water with ethyl acetate. The combined organic layers were washed with water and saturated aqueous sodium bicarbonate, dried (Na2SO4) and then concentrated under reduced pressure to give the title compound (3.0 g, 77%) as a brown solid: +APcI MS (M+1)+ 182; H NMR (CDCl3) δ: 6.74 (s, 1H), 6.42 (s, 1H), 2.55 (s, 3H), 2.53 (s, 3H).

المصدر