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Tetrahydrofuran → Benzyl 5-(3-ethoxy-2-ethoxy-3-oxo-1-propenyl)-2-methoxybenzoate

HRID 1816551
Notes
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Reaction equation

HRID 1816551 reaction equation
C(P([CH:7](CC)[C:8]([O:10][CH2:11][CH3:12])=[O:9])(CC)=O)C.[H-].[Na+].[CH:17]([C:19]1[CH:20]=[CH:21][C:22]([O:35][CH3:36])=[C:23]([CH:34]=1)[C:24]([O:26][CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)=[O:25])=O.[Cl-].[NH4+].[O:39]1CC[CH2:41][CH2:40]1>>[CH2:11]([O:10][C:8](=[O:9])[C:7]([O:39][CH2:40][CH3:41])=[CH:17][C:19]1[CH:20]=[CH:21][C:22]([O:35][CH3:36])=[C:23]([CH:34]=1)[C:24]([O:26][CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)=[O:25])[CH3:12]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

6

Reactant 5

HCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 22494010Ethyl 2-(diethylphosphoryl)-2-ethylacetateHCID 22494335Benzyl 5-formyl-2-methoxybenzoate

Product 1

HCID 69803661Benzyl 5-(3-ethoxy-2-ethoxy-3-oxo-1-propenyl)-2-methoxybenzoate

Procedure

1.5 g of ethyl 2-(diethylphosphoryl)-2-ethylacetate was dissolved in 30 ml tetrahydrofuran, and 0.26 g of 60% sodium hydride was added thereto under ice-cooling. The reaction solution was stirred for 30 minutes under ice-cooling and 1.5 g of benzyl 5-formyl-2-methoxybenzoate was added thereto, and the mixture was stirred at room temperature for 20 hours. Aqueous ammonium chloride solution was added to the reaction mixture, followed by extracting with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, and the solvent was evaporated. The residue was subjected to silica gel column chromatography, to give 1.6 g of benzyl 5-(3-ethoxy-2-ethoxy-3-oxo-1-propenyl)-2-methoxybenzoate as an E-Z mixture from fractions eluted with hexane-ethyl acetate (4:1).

Workup

  1. temperatureunder ice-cooling
  2. temperaturecooling
  3. stirringthe mixture was stirred at room temperature for 20 hours
  4. extractionby extracting with ethyl acetate
  5. washThe organic layer was washed with brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customthe solvent was evaporated

Sources & evidence

ORD record
ord-59d36ff3e2b34f3c8fcb3337d6e4b321
Source dataset
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06884821B1

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes