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Ethyl (2R)-2-methyl-5-(propan-2-ylidene)cyclopentane-1-carboxylate → Ethyl (2R)-2-methyl-5-oxocyclopentane-1-carboxylate

HRID 82344
Notes
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Reaction equation

HRID 82344 reaction equation
[CH3:1][C@@H:2]1[CH2:6][CH2:5][C:4](=C(C)C)[CH:3]1[C:10]([O:12][CH2:13][CH3:14])=[O:11].C(=O)=[O:16].C(O)(C)C>C(OCC)(=O)C>[CH3:1][C@@H:2]1[CH2:6][CH2:5][C:4](=[O:16])[CH:3]1[C:10]([O:12][CH2:13][CH3:14])=[O:11]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 11830361Ethyl (2R)-2-methyl-5-(propan-2-ylidene)cyclopentane-1-carboxylateHCID 86586944Isopropanol carbon dioxide

Product 1

HCID 11052075Ethyl (2R)-2-methyl-5-oxocyclopentane-1-carboxylateYield 96%

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

(2R)-Ethyl 2-methyl-5-(propan-2-ylidene)cyclopentanecarboxylate (24 g, 0.122 mol) in ethyl acetate (100 mL) was cooled to −68° C. with dry ice/isopropanol. Ozonized oxygen (5-7 ft3h−1 of O2) was bubbled through the solution for 3.5 hours. The reaction mixture was flushed with nitrogen at room temperature until the color disappeared. The ethyl acetate was removed under vacuum and the residue was dissolved in 150 mL of acetic acid and cooled by ice water. Then 45 g of zinc powder were added. The solution was stirred for 30 minutes and then filtered. The filtrate was neutralized with 2N NaOH (1.3 L) and NaHCO3. The aqueous phase was extracted with ether (3×200 mL). The organic phase was combined, washed with water, dried and concentrated to afford (2R)-ethyl 2-methyl-5-oxocyclopentanecarboxylate (20 g, 96%). 1H NMR (CDCl3, 400 MHz) δ 4.21 (m, 2H), 2.77 (d, J=11.2 Hz, 1H), 2.60 (m, 1H), 2.50-2.10 (m, 3H), 1.42 (m, 1H), 1.33 (m, 3H), 1.23 (m, 3H).

Workup

  1. customOzonized oxygen (5-7 ft3h−1 of O2) was bubbled through the solution for 3.5 hours
  2. customThe reaction mixture was flushed with nitrogen at room temperature until the color
  3. customThe ethyl acetate was removed under vacuum
  4. dissolutionthe residue was dissolved in 150 mL of acetic acid
  5. temperaturecooled by ice water
  6. additionThen 45 g of zinc powder were added
  7. filtrationfiltered
  8. extractionThe aqueous phase was extracted with ether (3×200 mL)
  9. washwashed with water
  10. customdried
  11. concentrationconcentrated

Sources & evidence

ORD record
ord-61342e832eb84bb19a55e5bcf531d3d4
Source dataset
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08846681B2

Reaction notes

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