반응 #2135255

반응 방정식

1-(3-Chloro-5-hydroxypyridin-2-yl)ethanone

bromo(methyl)magnesium

diethylether

bromo(methyl)magnesium

diethylether

sodium chloride

→

title compound

5-Chloro-6-(1-hydroxy-1-methylethyl)pyridin-3-ol

용매

THF

반응 조건

후처리

1. 1
   기타The mixture was degassed three times
2. 2
   workup.ADDITIONWhen the addition
3. 3
   workup.WAITit was left
4. 4
   온도to warm up to room temperature for 16 hours
5. 5
   추출it was extracted with EtOAc (2×10 mL)
6. 6
   건조dried over sodium sulfate
7. 7
   여과filtered
8. 8
   농축concentrated in vacuo

실험 절차

1-(3-Chloro-5-hydroxypyridin-2-yl)ethanone (0.075 g, 0.0068 mol) was dissolved in THF (2 mL). The mixture was degassed three times then cooled to 0° C. with an ice bath. Then bromo(methyl)magnesium in diethylether (0.3 mL, 0.0009 mol) was added dropwise to the reaction mixture under nitrogen keeping the temperature at 0° C. with an ice bath. When the addition was complete, it was left to warm up to room temperature for 16 hours. Then bromo(methyl)magnesium in diethylether (0.3 mL, 0.0009 mol) was added dropwise to the reaction mixture and was stirred at room temperature for further 3 hours. A saturated aqueous solution of sodium chloride was slowly added to the reaction mixture (10 mL) and then it was extracted with EtOAc (2×10 mL). The organic layers were combined, dried over sodium sulfate, filtered, and concentrated in vacuo to obtain the title compound as a translucent solid (0.049 g, 4% yield):

출처