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iso-Isopulegol → 1-(2-Hydroxy-4-methylcyclohexyl)ethanone, (1R,2S,4R)-

HRID 73196
Notes
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Reaction equation

HRID 73196 reaction equation
[C:1]([C@H:4]1[CH2:9][CH2:8][C@@H:7]([CH3:10])[CH2:6][C@@H:5]1[OH:11])(C)=[CH2:2].[O:12]=[O+][O-].O=O>C(Cl)Cl.CO>[OH:11][C@H:5]1[CH2:6][C@H:7]([CH3:10])[CH2:8][CH2:9][C@H:4]1[C:1](=[O:12])[CH3:2]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 2

HCID 11008146iso-IsopulegolHCID 131711318Oxygen ozone

Product 1

HCID 597523071-(2-Hydroxy-4-methylcyclohexyl)ethanone, (1R,2S,4R)-Yield 67%

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 6344DichloromethaneSolvent

Procedure

To the (1S,2R,5R)-2-Isopropenyl-5-methyl-cyclohexanol (2.07 g, 13.42 mmol) in DCM (67 mL) and MeOH (1.6 mL) at −78° C. was bubbled ozone/oxygen gas until the reaction mixture was turned blue and the excess ozone was flushed off with oxygen, Dimethyl sulfide (4.9 mL) was added at the same temperature, slowly warmed up to room temperature, stirred for over night, concentrated, purified on column chromatography using 10-20% EtOAc/hexane to give (1R,2S,4R)-1-(2-Hydroxy-4-methyl-cyclohexyl)-ethanone (1.40 g, 67%) as an oil. NMR 1H (CDCl3, 400 MHz): 4.29-4.27 ppm (m, 1H); 2.40-2.35 ppm (m, 1H); 2.19 ppm (s, 3H); 1.91-1.73 ppm (m, 5H); 1.05-0.91 ppm (m, 2H); 0.88 ppm (d, 3H).

Workup

  1. customthe excess ozone was flushed off with oxygen, Dimethyl sulfide (4.9 mL)
  2. additionwas added at the same temperature
  3. concentrationconcentrated
  4. custompurified on column chromatography

Sources & evidence

ORD record
ord-a9e9e8ed0c9f4d5a92667e4b0744d7d3
Source dataset
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08829030B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes