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

HRID 59798

반응식

HRID 59798 반응식
[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]

참가 물질

5

반응물 2

HCID 30914AcetylpyrazineHCID 517165Ammonium Acetate

생성물 1

HCID 185190061-(Pyrazin-2-yl)ethanamine수율 749%

시약·촉매·용매 2

HCID 5003444Sodium cyanoborohydride촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-37341f31c3054b56b8b8bd7b6fad65fe
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09440956B2

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