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

HRID 81002
Notes
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Reaction equation

HRID 81002 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 ft3h1 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 acetic acid (150 mL) and cooled by ice water. Zinc powder (45 g) was then 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 ft3h1 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 acetic acid (150 mL)
  5. temperaturecooled by ice water
  6. additionZinc powder (45 g) was then 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-558cd234add04293bc483278e4d6aaaf
Source dataset
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08846683B2

Reaction notes

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