Sulfuric Acid → HCID 54211560、化合物

HRID 397309

反応式

HRID 397309 の反応式
[CH3:1][C:2]([CH3:10])([CH3:9])[CH2:3][C@@H:4]([C:6]([OH:8])=[O:7])[NH2:5].S(=O)(=O)(O)O.[CH3:16][C:17](=[CH2:19])[CH3:18].[OH-].[Na+]>C(OCC)(=O)C.O1CCOCC1>[C:17]([O:7][C:6](=[O:8])[C@H:4]([CH2:3][C:2]([CH3:10])([CH3:9])[CH3:1])[NH2:5])([CH3:19])([CH3:18])[CH3:16]

参加物

7

反応物 4

HCID 1118Sulfuric AcidHCID 8255IsobutyleneHCID 14798Sodium Hydroxide2 回HCID 194032(2S)-2-Amino-4,4-dimethylpentanoic acid

生成物 1

HCID 54211560HCID 54211560、化合物収率 50.5%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 312751,4-Dioxane溶媒

実験手順

To a pressure bottle were added 1.5 gm (10.3 mMol) 4-methyl-(L)-leucine, 25 mL dioxane, 1.5 mL concentrated sulfuric acid and 25 mL isobutylene. The pressure bottle was stoppered and the reactants were shaken together for 18 hours. The reaction mixture was then treated with 60 mL cold 1N sodium hydroxide and 100 mL ethyl acetate. To this mixture was added sufficient 1N sodium hydroxide until the pH of the mixture was 8.5. The layers were separated and the aqueous phase was extracted well with ethyl acetate. The combined ethyl acetate phases were dried over sodium sulfate and concentrated under reduced pressure to provide an oil which gradually crystallized to provide 1.05 gm (50.5%) of the title compound.

後処理

  1. customThe layers were separated
  2. extractionthe aqueous phase was extracted well with ethyl acetate
  3. dry with materialThe combined ethyl acetate phases were dried over sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto provide an oil which
  6. customgradually crystallized

出典と根拠

ORDレコード
ord-5d9c1bd03b5242cc91317327f5a3abcb
出典データセット
uspto-grants-2003_08
特許番号
US06610680B1

関連ノート

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