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Sulfuric Acid → 4-Amino-4-methylpentanoic acid

HRID 851757
ノート
印刷プレビュー

反応式

HRID 851757 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 2280694-Amino-4-methylpentanoic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-52ea6fc441664654a6e13527b7f1c0a6
出典データセット
uspto-grants-1983_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04386103

反応ノート

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