HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium hydroxide, monohydrate → 4-(5-(Trifluoromethyl)isoxazol-3-yl)benzoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | 4-(5-Trifluoromethyl-isoxazol-3-yl)-benzoic acid ethyl ester | HCID 57606104 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 4-(5-(Trifluoromethyl)isoxazol-3-yl)benzoic acid | HCID 57606112 | 73.2% |
Reaction Steps
A solution of 4-(5-Trifluoromethyl-isoxazol-3-yl)-benzoic acid ethyl ester (Preparative Example 9, 2.25 g, 7.86 mmol) in THF (20 mL) was treated with an aqueous solution (5 mL) of lithium hydroxide monohydrate (660 mg, 15.72 mmol) and allowed to stir for 16 hr. The reaction was then evaporated to a small volume and treated with a 1 N aqueous hydrochloric acid solution (25 mL) and the resulting solids filtered, washed with water and air dried to afford product as a colorless solid (1.48 g, 73%). 1H NMR (DMSO-d6) 8.06 (s, 4 H), 8.13 (s, 1 H). 13C NMR 106.5, 118.0 (q, J=270), 127.9, 130.8, 131.2, 132.4, ˜150 quartet not resolved from baseline noise, 133.8, 162.8, 167.3. 19F NMR −63.6. LC/MS 6.04 min, [M+1]+ 258.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08921399B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-8320bc91c3844e919875866e4327fefc |
| Source note | uspto-grants-2014_12 |