Реакция #640960

Уравнение реакции

1-pyrazin-2-yl-ethanone

ammonium acetate

→

1-pyrazin-2-yl-ethylamine

Растворители

methanol

Условия реакции

Обработка

1. 1
   ДругоеAfter removal of methanol, water (20 mL)
2. 2
   workup.ADDITIONwas added to the residue
3. 3
   workup.ADDITIONthe resulting solution was basified by addition of sodium hydroxide to pH=13
4. 4
   ЭкстракцияThe aqueous solution was extracted with dichloromethane
5. 5
   Сушкаthe combined organic phase was dried over sodium sulfate
6. 6
   ДругоеRemoval of the solvent under reduced pressure

Методика

To a solution of 1-pyrazin-2-yl-ethanone (2.0 g, 15.85 mmol) and ammonium acetate (19.337 g, 158.5 mmol) in methanol (50 mL) was added sodium cyanoborohydride (0.7 g, 11.1 mmol) in one portion. The reaction mixture was stirred overnight at room temperature. After removal of methanol, water (20 mL) was added to the residue and the resulting solution was basified by addition of sodium hydroxide to pH=13. The aqueous solution was extracted with dichloromethane and the combined organic phase was dried over sodium sulfate. Removal of the solvent under reduced pressure afforded 14.62 g of 1-pyrazin-2-yl-ethylamine, yield: 75%. MS (M+H)=124.

Источник