HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 59641990, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Ethyl 2-oxocyclohexylacetate | HCID 91229 | — |
| Reactant | (2-Bromo-4-fluorophenyl)hydrazine hydrochloride | HCID 16370085 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 59641990 | HCID 59641990 | 29.5% |
Reaction Steps
To a suspension of 7.24 g of (2-bromo-4-fluorophenyl)hydrazine hydrochloric acid salt in 100 mL of acetic acid, 5.5 g of ethyl 2-(2-oxocyclohexyl)-acetate was added. The resulting mixture was heated to reflux for 1 h. Then 10 mL of ethanol was added and the reaction mixture was heated at reflux overnight. The solvent was evaporated and the residue was diluted with EtOAc and washed with saturated aqueous NaHCO3 solution, water, and brine successively. The organic layer was separated and dried over anhydrous sodium sulfate, filtered, and evaporated. The residue was purified by flash chromatography over silica gel (5% EtOAc/hexane) to afford 3.12 g of desired compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07618994B2 |
| Source dataset | uspto-grants-2009_11 |
| ORD ID | ord-9884cc138a63427184262aefebccb436 |
| Source note | uspto-grants-2009_11 |