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Potassium Carbonate → ethyl(2S)-3-{4-[2-(benzyloxy)-2-oxoethoxy]phenyl}-2-ethoxypropanoate

HRID 2109006
Notes
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Reaction equation

HRID 2109006 reaction equation
[CH2:1]([O:3][C@@H:4]([CH2:10][C:11]1[CH:16]=[CH:15][C:14]([OH:17])=[CH:13][CH:12]=1)[C:5]([O:7][CH2:8][CH3:9])=[O:6])[CH3:2].C(=O)([O-])[O-].[K+].[K+].Br[CH2:25][C:26]([O:28][CH2:29][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)=[O:27]>C(#N)C>[CH2:29]([O:28][C:26](=[O:27])[CH2:25][O:17][C:14]1[CH:13]=[CH:12][C:11]([CH2:10][C@H:4]([O:3][CH2:1][CH3:2])[C:5]([O:7][CH2:8][CH3:9])=[O:6])=[CH:16][CH:15]=1)[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 62576Benzyl bromoacetateHCID 9816147Ethyl (2S)-2-ethoxy-3-(4-hydroxyphenyl)propanoate

Product 1

HCID 11383604ethyl(2S)-3-{4-[2-(benzyloxy)-2-oxoethoxy]phenyl}-2-ethoxypropanoateYield 58%

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

To a solution of ethyl(2S)-2-ethoxy-3-(4-hydroxyphenyl)propanoate (23.8 g, 100 mmol, prepared as described in WO99/62872) in acetonitrile (200 mL) was added anhydrous potassium carbonate (31.9 g, 231 mmol) followed by benzyl bromoacetate (17.4 mL, 110 mmol) and the reaction mixture was refluxed overnight. The reaction mixture was allowed to cool to room temperature, insoluble salts were filtered off and the solution was concentrated in vacuo. The residue was taken up in ethyl acetate (300 mL), and the organic phase was washed with aqueous NaHCO3 (3×100 mL) and brine (100 mL), dried over anhydrous MgSO4, and concentrated in vacuo. Purification on silica gel with methylene chloride as the eluent and collection of pure fractions yielded 22.4 g (58%) of a yellow oil.

Workup

  1. temperaturethe reaction mixture was refluxed overnight
  2. filtrationinsoluble salts were filtered off
  3. concentrationthe solution was concentrated in vacuo
  4. washthe organic phase was washed with aqueous NaHCO3 (3×100 mL) and brine (100 mL)
  5. dry with materialdried over anhydrous MgSO4
  6. concentrationconcentrated in vacuo
  7. customPurification on silica gel with methylene chloride
  8. customas the eluent and collection of pure fractions

Sources & evidence

ORD record
ord-18a0057aecd441b09724f8144c402e52
Source dataset
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07514471B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes