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Sodium Hydroxide → Trans 4-(2-Chloro-4-fluoro-phenoxy)-3-hydroxy-piperidine-1-carboxylic acid tert-butyl ester

HRID 1714403
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HRID 1714403 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:14][CH2:13][C@@H:12]2[C@@H:10]([O:11]2)[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[Cl:15][C:16]1[CH:21]=[C:20]([F:22])[CH:19]=[CH:18][C:17]=1[OH:23].[OH-].[Na+].[Cl-].[NH4+]>O1CCOCC1.CCCCCCC.C(OCC)(=O)C>[C:1]([O:5][C:6]([N:8]1[CH2:14][CH2:13][C@@H:12]([O:23][C:17]2[CH:18]=[CH:19][C:20]([F:22])=[CH:21][C:16]=2[Cl:15])[C@H:10]([OH:11])[CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
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7

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HCID 14798Sodium HydroxideHCID 25517Ammonium ChlorideHCID 748142-Chloro-4-fluorophenolHCID 55273474tert-butyl (1S,6R)-7-oxa-3-azabicyclo[4.1.0]heptane-3-carboxylate

생성물 1

HCID 68506255Trans 4-(2-Chloro-4-fluoro-phenoxy)-3-hydroxy-piperidine-1-carboxylic acid tert-butyl ester

시약·촉매·용매 2

HCID 31275
1,4-Dioxane
용매
HCID 21899848Ethylacetate heptane용매2회

실험 절차

Rac-cis-7-Oxa-3-aza-bicyclo[4.1.0]heptane-3-carboxylic acid tert-butyl ester (1 g, 5 mmol) was solvated in dioxane (5 mL), 2-Chloro-4-Fluorophenol was added (1.471 g, 10 mmol) and sodium hydroxide (0.401 g, 10 mmol). After 20 hours refluxing, the mixture was cooled, ammonium chloride was added and the mixture extracted three times with ethyl acetate. The combined organic phases were dried with magnesium sulfate and concentrated under vacuum. After a flash chromatography with heptane/ethyl acetate 1:1 to 1:2 heptane/ethyl acetate a solid the title compound was obtained as solid (0.778 g, 45% yield). MS (m/e): 404.5 (M+AcO−).

후처리

  1. temperatureAfter 20 hours refluxing
  2. temperaturethe mixture was cooled
  3. extractionthe mixture extracted three times with ethyl acetate
  4. dry with materialThe combined organic phases were dried with magnesium sulfate
  5. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-0f043f77be3f4268a079654f59e3fdfa
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07795437B2

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