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Sodium Methoxide → (2S,3R)-3-(4-Benzyloxy-2-methyl-phenyl)-2-ethoxy-3-hydroxy-propionic acid methyl ester

HRID 1064878
Notes
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Reaction equation

HRID 1064878 reaction equation
[CH3:1][O-:2].[Na+].C([C@H]1COC(=O)N1[C:17](=[O:39])[C@@H:18]([O:36][CH2:37][CH3:38])[C@@H:19]([C:21]1[CH:26]=[CH:25][C:24]([O:27][CH2:28][C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)=[CH:23][C:22]=1[CH3:35])[OH:20])C1C=CC=CC=1>CO>[CH3:1][O:2][C:17](=[O:39])[C@@H:18]([O:36][CH2:37][CH3:38])[C@@H:19]([C:21]1[CH:26]=[CH:25][C:24]([O:27][CH2:28][C:29]2[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=2)=[CH:23][C:22]=1[CH3:35])[OH:20]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 10942334Sodium MethoxideHCID 68616303(S)-4-Benzyl-3-[(2S,3R)-3-(4-benzyloxy-2-methyl-phenyl)-2-ethoxy-3-hydroxy-propionyl]-oxazolidin-2-one

Product 1

HCID 68616209(2S,3R)-3-(4-Benzyloxy-2-methyl-phenyl)-2-ethoxy-3-hydroxy-propionic acid methyl esterYield 69.4%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A 5.4 M solution of sodium methoxide (7.3 ml, 39.5 mmol) was added to an ice-cooled and stirred suspension of (S)-4-benzyl-3-[(2S,3R)-3-(4-benzyloxy-2-methyl-phenyl)-2-ethoxy-3-hydroxy-propionyl]-oxazolidin-2-one (17.6 g, 36 mmol) in dry methanol (87 ml). The mixture was stirred at 0° C. for 15 min, quenched and neutralized by the addition of dilute aqueous hydrochloric acid (1.0 M). The solution was concentrated under reduced pressure and the residue dissolved in ice water/ethyl acetate 1/1. The layers were separated and the aqueous layer was extracted two times with ethyl acetate. The combined organic layers were washed with ice water and dried over sodium sulfate. The solvent was removed under reduced pressure and the residue purified by column chromatography (silica gel, cyclohexane/AcOEt) to give 8.6 g (25 mmol, 69%) of the title compound as light yellow oil. According to 1H-NMR spectroscopy, one single diastereomer was obtained.

Workup

  1. temperaturecooled
  2. stirringThe mixture was stirred at 0° C. for 15 min
  3. customquenched
  4. additionneutralized by the addition of dilute aqueous hydrochloric acid (1.0 M)
  5. concentrationThe solution was concentrated under reduced pressure
  6. dissolutionthe residue dissolved in ice water/ethyl acetate 1/1
  7. customThe layers were separated
  8. extractionthe aqueous layer was extracted two times with ethyl acetate
  9. washThe combined organic layers were washed with ice water
  10. dry with materialdried over sodium sulfate
  11. customThe solvent was removed under reduced pressure
  12. customthe residue purified by column chromatography (silica gel, cyclohexane/AcOEt)

Sources & evidence

ORD record
ord-f69a55dcd4d540ec828c90fb9059593e
Source dataset
uspto-grants-2005_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06969725B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes