HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diazomethane → Ethyl 3-cyclopropyl-4-fluorobenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diazomethane | HCID 9550 | — |
| Reactant | Ethyl 4-fluoro-3-vinylbenzoate | HCID 46941363 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | Ethyl 3-cyclopropyl-4-fluorobenzoate | HCID 40151794 | 99.1% |
Reaction Steps
To a mixture of ethyl 4-fluoro-3-vinylbenzoate (Preparation 54, 48 g, 0.25 mol, 1 eq) and palladium (II) acetate (2.5 g, 10 mmol, 0.4 eq) in ether (300 mL) was added diazomethane in ether (1.5 mol, 6.0 eq). Then the mixture was stirred at room temperature overnight. The reaction was quenched with a solution of AcOH (75 mL) in water (100 mL). The mixture was filtrated and the filtrate was added saturated solution of sodium carbonate until pH=10. The organic phase was washed with brine (200 mL) and water (200 mL), dried over sodium sulfate and concentrated in vacuo to give title compound as brown liquid (51 g, 0.248 mol, 99.1%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08741934B2 |
| Source dataset | uspto-grants-2014_06 |
| ORD ID | ord-c15e002275ee4bff9122cb558c695a60 |
| Source note | uspto-grants-2014_06 |