HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → Ethyl 2-[1-(2'-cyanobiphenyl-4-yl)ethyl]-3-oxohexanoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Ethyl 3-oxohexanoate | HCID 238498 | — |
| Reactant | 4'-(1-Bromoethyl)biphenyl-2-carbonitrile | HCID 67008558 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | Ethyl 2-[1-(2'-cyanobiphenyl-4-yl)ethyl]-3-oxohexanoate | HCID 67009459 | 94.2% |
Reaction Steps
To a mixture of 60% sodium hydride in oil (0.82 g) and tetrahydrofuran (20 mL) was added dropwise a mixture of ethyl 3-oxohexanoate (4.35 g) in tetrahydrofuran (20 mL) at 0° C., and the mixture was stirred at room temperature for 30 min. Then, 4′-(1-bromoethyl)biphenyl-2-carbonitrile (3.93 g) was added, and the mixture was stirred at 50° C. overnight. The reaction mixture was poured into 1 M hydrochloric acid (30 mL), and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography to give the title compound as a colorless oil (4.70 g, 94%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09115136B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-6d8d9dfea3554e49b5ba5159fe612cfd |
| Source note | uspto-grants-2015_08 |