HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 4-[5-(2-Methoxy-phenyl)-isoxazol-3-yl]-butyric acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1,4-Diisocyanatobenzene | HCID 61009 | — |
| Reactant | Methyl 5-nitropentanoate | HCID 543911 | — |
| Reactant | 1-Ethynyl-2-methoxybenzene | HCID 582912 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 4-[5-(2-Methoxy-phenyl)-isoxazol-3-yl]-butyric acid methyl ester | HCID 59167784 | 112.6% |
Reaction Steps
Add 1,4-phenylenediisocyanate (19.22 g, 120.0 mmol) to a stirred solution of 1-ethynyl-2-methoxy-benzene (2204901, 5.29 g, 40.0 mmol) and 5-nitro-pentanoic acid methyl ester (7.91 g, 49.1 mmol) in toluene (300 mL, anhydrous) and stir under N2. Add triethylamine (16.7 mL, 120.0 mmol) and heat to reflux under N2 overnight. Filter mixture through a pad of Celite® and rinse with toluene. Concentrate to get 12.4 g yellow oil. Adsorb on SiO2 and purify the residue by flash chromatography on silica gel eluting with 0-30% EtOAc/hexanes to afford the title compound (14.0 g, 74%). MS (IS) 276 (M+1)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07662771B2 |
| Source dataset | uspto-grants-2010_02 |
| ORD ID | ord-3439333d0c9b45aaaac5c4ab14b92823 |
| Source note | uspto-grants-2010_02 |