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Sulfuric Acid → 4-Amino-4-methylpentanoic acid

HRID 851757
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HRID 851757 반응식
[CH3:1][C:2]1([CH3:8])[NH:6][C:5](=[O:7])[CH2:4][CH2:3]1.[OH-].[Ba+2].[OH-].S(=O)(=O)(O)[OH:13].C(=O)([O-])[O-].[Ba+2]>O>[NH2:6][C:2]([CH3:8])([CH3:1])[CH2:3][CH2:4][C:5]([OH:13])=[O:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 1118Sulfuric AcidHCID 10563Barium CarbonateHCID 6093286Barium hydroxideHCID 111262105,5-Dimethylpyrrolidin-2-one

생성물 1

HCID 2280694-Amino-4-methylpentanoic acid

시약·촉매·용매 1

HCID 962Water용매

실험 절차

For example, a mixture of 5,5-dimethyl-2-pyrrolidone, an excess amount of barium hydroxide and a sufficient amount of water is heated under reflux until the reaction is substantially complete. The cooled solution is made slightly acidic with sulfuric acid and neutralized with solid barium carbonate or other bases. After removal of solids by filtration, the filtrate is evaporated under reduced pressure to yield a crude product which after three recrystallizations from an inert solvent such as aqueous ethanol gives an analytically pure product of 4-amino-4,4-dimethyl butanoic acid (4-amino-4-methylvaleric acid). 4-amino-2,4-dimethylvaleric acid is prepared similarly from 3,5,5-trimethyl-2-pyrrolidone.

후처리

  1. temperatureunder reflux until the reaction
  2. customAfter removal of solids
  3. filtrationby filtration
  4. customthe filtrate is evaporated under reduced pressure
  5. customto yield a crude product which
  6. customafter three recrystallizations from an inert solvent such as aqueous ethanol

출처 및 근거

ORD 기록
ord-52ea6fc441664654a6e13527b7f1c0a6
출처 데이터셋
uspto-grants-1983_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04386103

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