HuagongsheHuagongshe Chemistry Print Report · For research reference only
iso-Isopulegol → 1-(2-Hydroxy-4-methylcyclohexyl)ethanone, (1R,2S,4R)-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | iso-Isopulegol | HCID 11008146 | — |
| Reactant | Oxygen ozone | HCID 131711318 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1-(2-Hydroxy-4-methylcyclohexyl)ethanone, (1R,2S,4R)- | HCID 59752307 | 67% |
Reaction Steps
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).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08829030B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-a9e9e8ed0c9f4d5a92667e4b0744d7d3 |
| Source note | uspto-grants-2014_09 |