HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → Ethyl 3-(3-fluorophenyl)-5-methylisoxazole-4-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl 2-butynoate | HCID 78043 | — |
| Reactant | 3-fluoro-N-hydroxybenzene-1-carbonimidoyl chloride | HCID 14221338 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | Ethyl 3-(3-fluorophenyl)-5-methylisoxazole-4-carboxylate | HCID 22309060 | 39.5% |
Reaction Steps
To a solution of (E)- and/or (Z)—N-hydroxy-3-fluoro-benzenecarboximidoyl chloride (11.1 g, 64 mmol) in diethylether (151 mL) was added ethyl 2-butynoate (7.2 g, 7.5 mL, 64 mmol) at 0° C. followed by the dropwise addition of triethylamine (7.8 g, 10.7 mL, 77 mmol) and the resulting mixture allowed to warm up to room temperature overnight. The mixture was then poured onto ice-water, and extracted with diethylether. The combined organic layers were then washed with water and brine, dried over sodium sulfate and evaporated. Purification by chromatography (SiO2, heptane:ethyl acetate=100:0 to 1:1) afforded the title compound (6.3 g, 39%) which was obtained as a white solid. MS: m/e=250.1 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08877782B2 |
| Source dataset | uspto-grants-2014_11 |
| ORD ID | ord-03cb5ec63a3148678a88842435b42be4 |
| Source note | uspto-grants-2014_11 |