HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hexachloroethane → HCID 86731254, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hexachloroethane | HCID 6214 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 86731255 | HCID 86731255 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 86731254 | HCID 86731254 | 5.1% |
Reaction Steps
To a solution of 4-(cyclopropylmethoxy)-3-fluoro-N-(2-fluoro-4,6-dihydroxyphenyl)benzamide (2.29 g), hexachloroethane (4.04 g) and triphenylphosphine (4.48 g) in acetonitrile (50 mL) was added triethylamine (2.86 mL) at 0° C., and the mixture was stirred at room temperature for 15 min, and then with heating at 80° C. for 1 hr. The reaction mixture was filtered, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (110 mg). 1H NMR (300 MHz, CDCl3) δ 0.37-0.45 (2H, m), 0.65-0.74 (2H, m), 1.24-1.44 (1H, m), 3.97 (2H, d, J=7.2 Hz), 5.26 (1H, d, J=3.4 Hz), 6.97-7.10 (2H, m), 7.38 (1H, dd, J=8.5, 1.3 Hz), 7.87-7.98 (2H, m).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09133129B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-bc2a7013cca94f4883d72de914c87174 |
| Source note | uspto-grants-2015_09 |