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Diisopropylamine → 1-(4-Benzyloxy-2-tert-butoxycarbonylbutyl)cyclopentane carboxylic acid

HRID 1459888
Notes
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Reaction equation

HRID 1459888 reaction equation
C(NC(C)C)(C)C.C([Li])CCC.CCCCCC.[CH:19]1([C:24]([OH:26])=[O:25])[CH2:23][CH2:22][CH2:21][CH2:20]1.[C:27]([O:31][C:32](=[O:45])[C:33]([CH2:35][CH2:36][O:37][CH2:38][C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1)=[CH2:34])([CH3:30])([CH3:29])[CH3:28]>O1CCCC1>[CH2:38]([O:37][CH2:36][CH2:35][CH:33]([C:32]([O:31][C:27]([CH3:28])([CH3:30])[CH3:29])=[O:45])[CH2:34][C:19]1([C:24]([OH:26])=[O:25])[CH2:23][CH2:22][CH2:21][CH2:20]1)[C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 5

HCID 7912DiisopropylamineHCID 8058HexaneHCID 18840Cyclopentanecarboxylic acidHCID 539165622-(2-Benzyloxyethyl)acrylic acid tert-butyl esterHCID 178418339Butyllithium

Product 1

HCID 545513721-(4-Benzyloxy-2-tert-butoxycarbonylbutyl)cyclopentane carboxylic acid

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent3×

Conditions

Temperature
-40 °C

Procedure

To a solution of diisopropylamine (2.9 mL, 20.8 mmol) in dry tetrahydrofuran (50 mL) at -50° C. was added a 2.5M solution of n-butyllithium in hexane (8.4 mL, 21 mmol). The mixture was stirred at a temperature from -30° C. to 0° C. over 30 minutes and then cooled again to -40° C. A solution of cyclopentanecarboxylic acid (1.1 mL, 10.1 mmol) in tetrahydrofuran (20 mL) was added and the resulting mixture was allowed to warm to room temperature with stirring over 2 hours. The reaction was cooled to -79° C. and a solution of 2-(2-benzyloxyethyl) acrylic acid tert-butyl ester (2.6 g, 9.9 mmol) in dry tetrahydrofuran (10 mL) was added dropwise; stirring was continued at -40° C. for 2 hours. The mixture was quenched by the addition of 0.5M HCl solution and was extracted with ether. The extract was washed with brine, dried over MgSO4 and evaporated under vacuum to leave an oil from which 1-(4-benzyloxy-2-tert-butoxycarbonylbutyl)cyclopentane carboxylic acid, 2.9 g (78%), was isolated by chromatography on silica gel eluting with methylene chloride and then 1% methanol in methylene chloride.

Workup

  1. temperatureto warm to room temperature
  2. stirringwith stirring over 2 hours
  3. temperatureThe reaction was cooled to -79° C.
  4. stirringstirring
  5. waitwas continued at -40° C. for 2 hours
  6. customThe mixture was quenched by the addition of 0.5M HCl solution
  7. extractionwas extracted with ether
  8. washThe extract was washed with brine
  9. dry with materialdried over MgSO4
  10. customevaporated under vacuum

Sources & evidence

ORD record
ord-d322f8958c3e40bebff669be2da5413c
Source dataset
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05854275

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes