반응 #11946

반응 방정식

5-methylpyrazine 2-carboxylic acid

methanol

chlorine

→

title compound

2-methoxycarbonyl-5-methylpyrazine

반응 조건

후처리

1. 1
   농축the reaction solution was concentrated
2. 2
   workup.ADDITION1 mol/l aqueous solution of sodium hydroxide was added
3. 3
   추출followed by extraction with chloroform
4. 4
   세척The organic layer was washed with saturated brine
5. 5
   건조dried over anhydrous sodium sulfate
6. 6
   농축concentrated
7. 7
   기타The resulting solid was recrystallized from hexane/ethyl acetate
8. 8
   여과The deposited crystals were collected by filtration
9. 9
   기타dried under reduced pressure

실험 절차

Commercially available 5-methylpyrazine 2-carboxylic acid (2.05 g) was dissolved in methanol (0.6 ml) and chlorine gas was blown into the solution for 5 minutes. After four hours, the reaction solution was concentrated and 1 mol/l aqueous solution of sodium hydroxide was added, followed by extraction with chloroform. The organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated. The resulting solid was recrystallized from hexane/ethyl acetate. The deposited crystals were collected by filtration and dried under reduced pressure to obtain the title compound (1.44 g) as light brown scale-like crystals.

출처