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Sodium Hydroxide → 1-Benzyl-4-methylpyrrolidin-3-amine

HRID 358909
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HRID 358909 반응식
[OH-].[Na+].[CH2:3]([N:10]1[CH2:14][CH:13]([CH3:15])[C:12](=[N:16]O)[CH2:11]1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1>C(O)C.[Ni]>[CH2:3]([N:10]1[CH2:14][CH:13]([CH3:15])[CH:12]([NH2:16])[CH2:11]1)[C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 859932571-Benzyl-3-(hydroxyimino)-4-methylpyrrolidine

생성물 1

HCID 142112411-Benzyl-4-methylpyrrolidin-3-amine수율 712.6%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

실험 절차

90 ml of a 20% w/v aqueous solution of sodium hydroxide were added to a solution of 12 g (0.059 mole) of 1-benzyl-3-(hydroxyimino)-4-methylpyrrolidine [prepared as described in Step (5) above] dissolved in 100 ml of ethanol. 23.9 g of Raney nickel (about 50%) were gradually added to the mixture, whilst vigorously stirring it. After the reaction mixture had been stirred for 3 hours, it was filtered. The upper layer of the filtrate was separated and concentrated by evaporation under reduced pressure. The residue was purified by column chromatography through silica gel eluted with methanol, to give 80 g of 1-benzyl-3-amino-4-methylpyrrolidine as a pale yellow liquid.

후처리

  1. stirringAfter the reaction mixture had been stirred for 3 hours
  2. filtrationit was filtered
  3. customThe upper layer of the filtrate was separated
  4. concentrationconcentrated by evaporation under reduced pressure
  5. customThe residue was purified by column chromatography through silica gel
  6. washeluted with methanol

출처 및 근거

ORD 기록
ord-dfc7eee44f354ab08a1dd587cccbb18a
출처 데이터셋
uspto-grants-1991_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04997943

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