HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 57184026, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | HCID 54282312 | HCID 54282312 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 57184026 | HCID 57184026 | 92.5% |
Reaction Steps
4 g of (1R)-3,3,5-trimethyl-4-methylene-1-cyclohexanol obtained in Example 2A were dissolved in 50 ml of toluene, about 6 mg of p-toluenesulfonic acid were added and the mixture was refluxed for 45 min. It was then poured into 50 ml of water and extracted twice with 50 ml of ether. The organic phase was separated off, washed with 50 ml of saturated NaHCO3 solution, dried over MgSO4 and freed of solvent under reduced pressure. The residue was chromatographed on 150 g of silica gel with hexane/EA (4:1) to result in 3.7 g of the abovementioned product in the form of pale yellow crystals with a purity of 97% according to GC.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06111125 |
| Source dataset | uspto-grants-2000_08 |
| ORD ID | ord-1fbd0de7bbae411299ef4245c0d14a52 |
| Source note | uspto-grants-2000_08 |