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Acetic Acid → ethyl (3S,4S)-4-{[(benzyloxy)carbonyl]amino}-3-hydroxy-5-methylhexanoate

HRID 2046656
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HRID 2046656 반응식
C(N[CH:5]([CH3:7])[CH3:6])(C)C.C([Li])CCC.[C:13]([O:16][CH2:17][CH3:18])(=[O:15])[CH3:14].[CH:19]([C@@H:21]([NH:25][C:26](=[O:35])[O:27][CH2:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)[CH:22]([CH3:24])[CH3:23])=[O:20].[C:36]([OH:39])(=[O:38])[CH3:37]>O1CCCC1.CCCCCC.O>[CH2:28]([O:27][C:26]([NH:25][C@@H:21]([CH:22]([CH3:24])[CH3:23])[C@@H:19]([OH:20])[CH2:14][C:13]([O:16][CH2:17][CH3:18])=[O:15])=[O:35])[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1.[CH2:28]([O:27][C:26]([NH:25][CH:37]([CH:13]([OH:15])[CH2:14][CH:5]([CH3:6])[CH3:7])[C:36]([O-:39])=[O:38])=[O:35])[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1
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참가 물질

10

반응물 5

HCID 176Acetic AcidHCID 7912DiisopropylamineHCID 8857Ethyl AcetateHCID 11009915benzyl [(1S)-1-formyl-2-methylpropyl]carbamateHCID 178418339Butyllithium

생성물 2

HCID 59370506ethyl (3S,4S)-4-{[(benzyloxy)carbonyl]amino}-3-hydroxy-5-methylhexanoate
HCID 131731055
([(Benzyloxy)carbonyl]amino}-3-hydroxy-5-methylhexanoate

시약·촉매·용매 3

HCID 962Water용매HCID 8028Tetrahydrofuran용매3회HCID 8058Hexane용매

반응 조건

온도
-78 °C

실험 절차

To a solution (40 mL) of diisopropylamine (4.6 mL) in tetrahydrofuran was added 1.6 mol/L solution (20.19 mL) of n-butyllithium in hexane, and the mixture was cooled to −78° C. A solution (5 mL) of ethyl acetate (3.16 mL) in tetrahydrofuran was added dropwise to the mixture at a rate to maintain the reaction mixture at −70° C. or below. After the completion of the dropwise addition, the mixture was stirred at −78° C. for 1 hr, a solution (10 mL) of benzyl [(1S)-1-formyl-2-methylpropyl]carbamate (1.9 g) in tetrahydrofuran was added dropwise thereto at a rate to maintain the reaction mixture at −70° C. or below. The reaction mixture was once warmed to −30° C., and cooled again to −78° C. Acetic acid (2.3 mL) was added to the mixture, and the temperature of the mixture was raised to room temperature. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (developing solvent: hexane:ethyl acetate=9:1→2:1) to give the title compound (yield: 800 mg) and ethyl (3R,4S)-4-{([(benzyloxy)carbonyl]amino}-3-hydroxy-5-methylhexanoate (yield: 550 mg) both as a colorless oil.

후처리

  1. temperatureto maintain the reaction mixture at −70° C. or below
  2. additionAfter the completion of the dropwise addition
  3. temperatureat a rate to maintain the reaction mixture at −70° C. or below
  4. temperatureThe reaction mixture was once warmed to −30° C.
  5. temperaturecooled again to −78° C
  6. temperaturethe temperature of the mixture was raised to room temperature
  7. extractionthe mixture was extracted with ethyl acetate
  8. washThe extract was washed with saturated brine
  9. dry with materialdried over anhydrous sodium sulfate
  10. concentrationconcentrated under reduced pressure
  11. customThe residue was purified by silica gel column chromatography (developing solvent: hexane:ethyl acetate=9:1→2:1)

출처 및 근거

ORD 기록
ord-972484da68c24c768cbd3f837d393ee4
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08592452B2

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