반응 #85113

반응 방정식

pyridinium hydrobromide

4-bromo-2,5-dimethoxypyridine

→

4-Bromo-5-methoxypyridin-2(1H)-one

용매

dimethylformamide

반응 조건

후처리

1. 1
   농축concentrated under reduced pressure
2. 2
   기타The residue was triturated with 50 ml of water
3. 3
   여과filtered off
4. 4
   세척washed with water
5. 5
   기타dried under reduced pressure
6. 6
   추출The filtrate was extracted twice with dichloromethane/methanol (10:1)
7. 7
   건조The combined organic phases were dried (sodium sulphate)
8. 8
   여과filtered
9. 9
   농축concentrated under reduced pressure
10. 10
    기타dried

실험 절차

2.82 g (176 mmol, 20 eq.) of pyridinium hydrobromide were added to a solution of 1.94 g (8.81 mmol) of 4-bromo-2,5-dimethoxypyridine in 80 ml of dimethylformamide, the mixture was stirred at 100° C. for 3 h and concentrated under reduced pressure. The residue was triturated with 50 ml of water, filtered off, washed with water and dried under reduced pressure. The filtrate was extracted twice with dichloromethane/methanol (10:1). The combined organic phases were dried (sodium sulphate), filtered, concentrated under reduced pressure and dried. Yield: 771 mg (43% of theory) and 465 mg (purity 88%, 23% of theory)

출처