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

HRID 59798

反応式

HRID 59798 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 749%

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-37341f31c3054b56b8b8bd7b6fad65fe
出典データセット
uspto-grants-2016_09
特許番号
US09440956B2

関連ノート

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