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Sodium Hydroxide → HCID 57893118, 화합물

HRID 1511455
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HRID 1511455 반응식
C([O:4][CH:5]([C@@H:12]([NH:18][C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])[CH2:13][CH:14]1[CH2:17][CH2:16][CH2:15]1)[C:6]([NH:8][CH:9]1[CH2:11][CH2:10]1)=[O:7])(=O)C.[OH-].[Na+]>CO>[CH:14]1([CH2:13][C@H:12]([NH:18][C:19](=[O:20])[O:21][C:22]([CH3:24])([CH3:23])[CH3:25])[CH:5]([OH:4])[C:6]([NH:8][CH:9]2[CH2:10][CH2:11]2)=[O:7])[CH2:17][CH2:16][CH2:15]1
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참가 물질

4

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HCID 14798Sodium HydroxideHCID 57893114(3S)-3-(tert-butoxycarbonylamino)-4-cyclobutyl-1-(cyclopropylamino)-1-oxobutan-2-yl acetate

생성물 1

HCID 57893118HCID 57893118, 화합물수율 86.8%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of (3S)-3-(tert-butoxycarbonylamino)-4-cyclobutyl-1-(cyclopropylamino)-1-oxobutan-2-yl acetate (3.8 g, 10.7 mmol) in methanol (50 mL) was added sodium hydroxide aqueous solution (1N, 15 mL) at room temperature. After 2 hours, methanol was removed under reduced pressure, and the concentrate was extracted with ethyl acetate. The ethyl acetate was washed with brine and dried over magnesium sulfate. The solvent was removed under reduced pressure, and the residue was crystallized from 100 mL of ethyl acetate and hexane(v/v=3/1) to give tert-butyl (2S)-1-cyclobutyl-4-(cyclopropylamino)-3-hydroxy-4-oxobutan-2-ylcarbamate (2.9 g) as a white solid.

후처리

  1. custommethanol was removed under reduced pressure
  2. extractionthe concentrate was extracted with ethyl acetate
  3. washThe ethyl acetate was washed with brine
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was removed under reduced pressure
  6. customthe residue was crystallized from 100 mL of ethyl acetate and hexane(v/v=3/1)

출처 및 근거

ORD 기록
ord-8c8c298723ee4e1db462305b31f299cd
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08211897B2

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