Sulfuric Acid → HCID 54211560, 화합물

HRID 397309노트

반응식

HRID 397309 반응식
[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]

참가 물질

7

반응물 4

HCID 1118Sulfuric AcidHCID 8255IsobutyleneHCID 14798Sodium Hydroxide2회HCID 194032(2S)-2-Amino-4,4-dimethylpentanoic acid

생성물 1

HCID 54211560HCID 54211560, 화합물수율 50.5%

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5d9c1bd03b5242cc91317327f5a3abcb
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06610680B1

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