تفاعل #11946

معادلة التفاعل

5-methylpyrazine 2-carboxylic acid

methanol

chlorine

→

title compound

2-methoxycarbonyl-5-methylpyrazine

ظروف التفاعل

المعالجة

1. 1
   تركيزthe reaction solution was concentrated
2. 2
   workup.ADDITION1 mol/l aqueous solution of sodium hydroxide was added
3. 3
   استخلاصfollowed by extraction with chloroform
4. 4
   غسيلThe organic layer was washed with saturated brine
5. 5
   تجفيفdried over anhydrous sodium sulfate
6. 6
   تركيزconcentrated
7. 7
   أخرىThe resulting solid was recrystallized from hexane/ethyl acetate
8. 8
   ترشيحThe deposited crystals were collected by filtration
9. 9
   أخرىdried under reduced pressure

الإجراء التجريبي

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.

المصدر