反応 #1757050

反応方程式

1-pyrazin-2-yl-ethanone

ammonium acetate

→

1-pyrazin-2-yl-ethylamine

溶媒

methanol

反応条件

後処理

1. 1
   その他After 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
   抽出The aqueous solution was extracted with dicholromethane
5. 5
   乾燥the combined organic phase was dried over sodium sulfate
6. 6
   その他Removal of the solvent under reduced pressure

実験手順

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 dicholromethane 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.

出典