Acetylpyrazine → 1-(Pyrazin-2-yl)ethanamine

HRID 77761

反応式

HRID 77761 の反応式
[N:1]1[CH:6]=[CH:5][N:4]=[CH:3][C:2]=1[C:7](=O)[CH3:8].C([O-])(=O)C.[NH4+:14]>CO.C([BH3-])#N.[Na+]>[N:1]1[CH:6]=[CH:5][N:4]=[CH:3][C:2]=1[CH:7]([NH2:14])[CH3:8]

参加物

5

反応物 2

HCID 30914AcetylpyrazineHCID 517165Ammonium Acetate

生成物 1

HCID 185190061-(Pyrazin-2-yl)ethanamine収率 2,374.2%

試薬・触媒・溶媒 2

HCID 5003444Sodium cyanoborohydride触媒HCID 887Methanol溶媒

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.

後処理

  1. customAfter removal of methanol, water (20 mL)
  2. additionwas added to the residue
  3. additionthe resulting solution was basified by addition of sodium hydroxide to pH=13
  4. extractionThe aqueous solution was extracted with dicholromethane
  5. dry with materialthe combined organic phase was dried over sodium sulfate
  6. customRemoval of the solvent under reduced pressure

出典と根拠

ORDレコード
ord-7f2d10cabd6c4543b0705e4dffba92dd
出典データセット
uspto-grants-2014_09
特許番号
US08841336B2

関連ノート

読み込み中…