HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 68527500, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Reactant | HCID 68524570 | HCID 68524570 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 68527500 | HCID 68527500 | 97.3% |
Reaction Steps
To a suspension of 6-(1-hydroxy-cyclohexyl)-pyridin-3-ol (2.5 g, 12.9 mmol) in toluene (130 mL) was added p-toluenesulfonic acid monohydrate (8.12 g, 42.7 mmol). The mixture was refluxed with azeotropic removal of water for 2 hours. The reaction mixture was cooled to room temperature, neutralized with aqueous NaHCO3 and extracted three times with EtOAc. The organic phase was washed with brine, dried (Na2SO4), passed through a silica gel pad and concentrated to provide the title compound as a solid (2.2 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08642603B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-b0ecb34658784caea30c2fbf5e0ba749 |
| Source note | uspto-grants-2014_02 |