HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 54499309, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 2-Hydroxy-1-(4-methoxyphenyl)ethanone | HCID 77786 | — |
| Reactant | HCID 86757140 | HCID 86757140 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 54499309 | HCID 54499309 | 78.8% |
Reaction Steps
To a solution of 17.62 g of 2-hydroxy-4′-methoxyacetophenone (Kovach et al., J. Amer. Chem. Soc., Vol. 115, No. 23, (1993) p. 10476) and 12.96 g of pyridine in 240 ml of dichloromethane, a solution of 26.32 g of eugenol-chloroformate in 60 ml of dichloromethane was dropped in at 5-10° C. Then, the mixture was stirred for 6 hours at room temperature. The reaction mixture was then acidified with 2N HCl and extracted with ether. The combined organic phases were washed with 2N HCl, saturated sodium bicarbonate and brine, and then dried, filtered, and evaporated to dryness. The resulting solid was purified by recrystallization to yield 29.79 g of yellow crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06258854B1 |
| Source dataset | uspto-grants-2001_07 |
| ORD ID | ord-d841b6e27acd447797caa918cceffa55 |
| Source note | uspto-grants-2001_07 |