HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methylmorpholine → HCID 86649956, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methylmorpholine | HCID 7972 | — |
| Reactant | N,O-Dimethylhydroxylamine | HCID 14232 | — |
| Reactant | 4-(4,6-Dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride | HCID 2734059 | — |
| Reactant | 2-Propoxy-4-(trifluoromethyl)benzoic acid | HCID 22494192 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86649956 | HCID 86649956 | 49.3% |
Reaction Steps
2-Propoxy-4-(trifluoromethyl)benzoic acid (457 mg, 1.93 mmol) in THF was reacted with N,O-dimethylhydroxy amine (378 mg), NMM (0.65 ml) and DMTMM (947 mg) at room temperature overnight. The reaction solvent was removed in vacuo. Water (30 ml) was added to the resulting residue, which was extracted with ethyl acetate (30 ml×3). The combined organic layer was washed with 1 M NaHCO3 (30 ml), 1N HCl (30 ml) and brine (30 ml) and dried over MgSO4. The filterate was purified with column chromatography (Hex/EtOAc=4/1) to yield the title compound (277 mg, 49%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08557872B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-5987c93a87ff4f308489e1355f8dac77 |
| Source note | uspto-grants-2013_10 |