HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Chloride → 5-(5-Fluoro-2-methoxyphenyl)-5-methyl-2-(2-methylquinolin-5-ylimino)-3-(trifluoromethyl)hexan-3-ol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Chloride | HCID 5234 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 5-Quinolinamine, 2-methyl- | HCID 148683 | — |
| Reactant | 5-(5-Fluoro-2-methoxyphenyl)-3-hydroxy-5-methyl-3-(trifluoromethyl)hexan-2-one | HCID 21948828 | — |
| Catalyst | Titanium | HCID 23963 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 5-(5-Fluoro-2-methoxyphenyl)-5-methyl-2-(2-methylquinolin-5-ylimino)-3-(trifluoromethyl)hexan-3-ol | HCID 21948924 | 62.5% |
Reaction Steps
645 mg (2 mmol) of 5-(5-fluoro-2-methoxyphenyl)-3-hydroxy-5-methyl-3-(trifluoromethyl)hexan-2-one is refluxed in 4 ml of tetrahydrofuran under nitrogen with 0.84 ml (4 mmol) of titanium tetraethylate and 348 mg (2.2 mmol) of 5-amino-2-methylquinoline for 24 hours. After cooling to room temperature, the reaction mixture is stirred into 20 ml of saturated NaCl solution, 50 ml of ethyl acetate is added, and it is stirred for 30 minutes, suctioned off on Celite, and rewashed with ethyl acetate and with tetrahydrofuran. The organic phase is separated, dried (sodium sulfate) and concentrated by evaporation. Chromatography on silica gel with hexane-ethyl acetate yields 578 mg of the product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07109212B2 |
| Source dataset | uspto-grants-2006_09 |
| ORD ID | ord-f8c19f4287b3492dbc5eaeeec179e92c |
| Source note | uspto-grants-2006_09 |