反応 #11946

反応方程式

5-methylpyrazine 2-carboxylic acid

methanol

chlorine

→

title compound

2-methoxycarbonyl-5-methylpyrazine

反応条件

後処理

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

実験手順

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.

出典