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Hydrochloric Acid → [(3S,5R)-5-(3,4,5-trifluorophenyl)morpholin-3-yl]methanol

HRID 553957
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HRID 553957 반응식
Cl.C([O:9][CH2:10][C@H:11]([NH:26]C(=O)OC(C)(C)C)[CH2:12][O:13][CH2:14][C:15](=O)[C:16]1[CH:21]=[C:20]([F:22])[C:19]([F:23])=[C:18]([F:24])[CH:17]=1)C1C=CC=CC=1>C(OCC)(=O)C>[F:24][C:18]1[CH:17]=[C:16]([C@H:15]2[NH:26][C@@H:11]([CH2:10][OH:9])[CH2:12][O:13][CH2:14]2)[CH:21]=[C:20]([F:22])[C:19]=1[F:23]
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 67373700tert-butyl {(S)-1-benzyloxymethyl-2-[2-oxo-2-(3,4,5-trifluorophenyl)ethoxy]ethyl}carbamate

생성물 1

HCID 67373759[(3S,5R)-5-(3,4,5-trifluorophenyl)morpholin-3-yl]methanol수율 78.5%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

A solution of 4 N hydrochloric acid in ethyl acetate (30 mL) was added to a solution of tert-butyl {(S)-1-benzyloxymethyl-2-[2-oxo-2-(3,4,5-trifluorophenyl)ethoxy]ethyl}carbamate (3.55 g) in ethyl acetate (30 mL) at room temperature. The reaction solution was stirred at room temperature for one hour and then concentrated under reduced pressure. 10% palladium-carbon (containing 50% water, 167 mg) was added to a solution of the resulting residue in methanol (50 mL), and the reaction solution was stirred in a hydrogen atmosphere at room temperature for 18 hours. Palladium-carbon in the reaction solution was removed by filtration, and then the filtrate was concentrated under reduced pressure. A saturated sodium bicarbonate solution and ethyl acetate were added to the resulting residue, and the organic layer was separated. The organic layer was washed with brine. The resulting organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (elution solvent: heptane-ethyl acetate system) to obtain 1.52 g of the title compound. The property values of the compound are as follows.

후처리

  1. concentrationconcentrated under reduced pressure
  2. addition10% palladium-carbon (containing 50% water, 167 mg) was added to a solution of the resulting residue in methanol (50 mL)
  3. stirringthe reaction solution was stirred in a hydrogen atmosphere at room temperature for 18 hours
  4. customPalladium-carbon in the reaction solution was removed by filtration
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. additionA saturated sodium bicarbonate solution and ethyl acetate were added to the resulting residue
  7. customthe organic layer was separated
  8. washThe organic layer was washed with brine
  9. dry with materialThe resulting organic layer was dried over anhydrous magnesium sulfate
  10. concentrationconcentrated under reduced pressure
  11. customThe residue was purified by silica gel column chromatography (elution solvent: heptane-ethyl acetate system)

출처 및 근거

ORD 기록
ord-6fa2826ce7c5463b943432b8891bd6b8
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08048878B2

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