HuagongsheHuagongshe Chemistry Print Report · For research reference only
Carbon Tetrachloride → HCID 44184988, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Carbon Tetrachloride | HCID 5943 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 58653729 | HCID 58653729 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 44184988 | HCID 44184988 | 89.1% |
Reaction Steps
4-(5-Fluoro-2-hydroxy-3-(2-hydroxyethyl)phenyl)-2-hydroxy-4-methyl-2-trifluoromethyl-valeric acid ethyl ester (3.90 g, 10.2 mmol) is dissolved with triphenylphosphine (3.14 g, 12 mmol) and triethylamine (2.1 ml, 15 mmol) in acetonitrile (150 ml), mixed with carbon tetrachloride (2 ml) and stirred for 3 days in a nitrogen atmosphere at room temperature. The solvent is distilled off in a rotary evaporator, and the residue is taken up in ethyl acetate (150 ml) and water (75 ml). The ethyl acetate phase is separated, washed with saturated NaCl solution, dried (Na2SO4) and concentrated by evaporation in a vacuum. Column chromatography on silica gel with hexane-ethyl acetate yields 3.31 g of the product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07417056B2 |
| Source dataset | uspto-grants-2008_08 |
| ORD ID | ord-6bd5bd39716c4934b4bf8821a53f5aa1 |
| Source note | uspto-grants-2008_08 |