HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methylmorpholine → HCID 86649958, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methylmorpholine | HCID 7972 | — |
| Reactant | N,O-Dimethylhydroxylamine | HCID 14232 | — |
| Reactant | 2-Nitro-4-(trifluoromethyl)benzoic acid | HCID 642096 | — |
| Reactant | 4-(4,6-Dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride | HCID 2734059 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86649958 | HCID 86649958 | 87.3% |
Reaction Steps
2-Nitro-4-trifluoromethyl-benzoic acid (2.753 mg, 11.7 mmol) in THF was reacted with N,O-dimethylhydroxy amine (1.277 g, 13.1 mmol), NMM (3 ml) and DMTMM (3.34 g) at room temperature overnight. The reaction mixture was quenched by adding H2O. The mixture was extracted with ethyl acetate (50 ml×3). The combined organic layer was washed 1M NaHCO3 (50 ml×2), 3% HCl (50 ml×2) and brine (50 ml), and then dried over MgSO4. The filterate was concentrated in vacuo to yield the title compound (2.84 g, 87%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08557872B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-dc3274863bd7483eb60ae0cc122336b1 |
| Source note | uspto-grants-2013_10 |