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Lithium Hydroxide → Rac-trans-cyclopentane-1,2-dicarboxylic acid monoethyl ester

HRID 557716
Notes
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Reaction equation

HRID 557716 reaction equation
[CH2:1]([O:3][C:4]([C@@H:6]1[CH2:10][CH2:9][CH2:8][C@H:7]1[C:11]([O:13]CC)=[O:12])=[O:5])[CH3:2].[OH-].[Li+]>O>[CH2:1]([O:3][C:4]([C@@H:6]1[CH2:10][CH2:9][CH2:8][C@H:7]1[C:11]([OH:13])=[O:12])=[O:5])[CH3:2]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 3939Lithium HydroxideHCID 57377009diethyl (1R,2R)-cyclopentane-1,2-dicarboxylate

Product 1

HCID 57652016Rac-trans-cyclopentane-1,2-dicarboxylic acid monoethyl esterYield 27.7%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

To a solution of rac-trans-cyclopentane-1,2-dicarboxylic acid diethyl ester (393 mg, 1.84 mmol) was added a solution of lithium hydroxide (75.5 mg, 1.8 mmol) in water (7 mL). The reaction mixture was stirred at room temperature for 30 minutes and then heated to 55° C. for 1 hr. The reaction mixture was cooled and evaporated under reduced pressure. The residue was dissolved in 25 mL water and washed with diethyl ether (2×5 mL). The pH of the aqueous layer was adjusted to pH 5 with 1N hydrochloric acid and extracted with methylene chloride (2×5 mL) and ethyl acetate (5 mL). The combined organic layers were dried over magnesium sulfate, filtered and evaporated to dryness under vacuum to give rac-trans-cyclopentane-1,2-dicarboxylic acid monoethyl ester (95 mg) that was used without further purification.

Workup

  1. temperatureheated to 55° C. for 1 hr
  2. temperatureThe reaction mixture was cooled
  3. customevaporated under reduced pressure
  4. dissolutionThe residue was dissolved in 25 mL water
  5. washwashed with diethyl ether (2×5 mL)
  6. extractionextracted with methylene chloride (2×5 mL) and ethyl acetate (5 mL)
  7. dry with materialThe combined organic layers were dried over magnesium sulfate
  8. filtrationfiltered
  9. customevaporated to dryness under vacuum

Sources & evidence

ORD record
ord-82bd7d6151a149cc990d0998bb18f995
Source dataset
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08058299B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes