HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Mercaptoethanol → HCID 19430498, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Mercaptoethanol | HCID 1567 | — |
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | 1-(4-Chlorophenyl)-2-(1H-1,2,4-triazol-1-yl)ethan-1-one | HCID 716472 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Cyclohexane | HCID 8078 | — |
| Product | HCID 19430498 | HCID 19430498 | 27.9% |
Reaction Steps
To a slurry of 44.3 g 1-(4-chlorophenyl)-2-(1H-1,2,4-triazol-l-yl) ethanone in 800 ml dry toluene and 400 ml 1-butanol was added 31.2 g 2-mercaptoethanol and 51.0 g p-toluenesulfonic acid. The mixture was refluxed under a Dean-Stark trap for 48 hours. On cooling, a white solid precipitated out, which was removed by filtration. The filtrate was evaporated, the residue dissolved in dichloromethane and washed twice with 10% aqueous sodium hydroxide and once with water. The organic layer was dried, filtered and evaporated to leave an oil which was taken up in cyclohexane. The cyclohexane was evaporated to azeotrope off any remaining 1-butanol, leaving an oily solid which was triturated with petroleum ether to give 15.7 g of product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05039332 |
| Source dataset | uspto-grants-1991_08 |
| ORD ID | ord-7a6e5a28465342498b62ad9f3337bc68 |
| Source note | uspto-grants-1991_08 |