反应 #11946

反应方程式

5-methylpyrazine 2-carboxylic acid

methanol

chlorine

→

title compound

2-methoxycarbonyl-5-methylpyrazine

反应条件

后处理

1. 1
   浓缩the reaction solution was concentrated
2. 2
   workup.ADDITION1 mol/l aqueous solution of sodium hydroxide was added
3. 3
   萃取followed by extraction with chloroform
4. 4
   洗涤The organic layer was washed with saturated brine
5. 5
   干燥dried over anhydrous sodium sulfate
6. 6
   浓缩concentrated
7. 7
   其他The resulting solid was recrystallized from hexane/ethyl acetate
8. 8
   过滤The deposited crystals were collected by filtration
9. 9
   其他dried under reduced pressure

实验过程

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.

来源