HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 178502659, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | O-methylhydroxylammonium chloride | HCID 11639 | — |
| Reactant | HCID 70155832 | HCID 70155832 | — |
| Solvent | Isobutanol | HCID 6560 | — |
| Product | HCID 178502659 | HCID 178502659 | 31.1% |
Reaction Steps
To 3 ml of isobutyl alcohol was added 0.75 g (0.0033 mole) of 1-methylthio-1-(3-pyridylmethyl)amino-2-nitroethylene, followed by addition of 0.56 g of 0-methylhydroxylamine hydrochloride at 100-110° C. Then, a solution of 0.93 ml of triethylamine in 1 ml of isobutyl alcohol was added dropwise at the same temperature with stirring over a period of 30 minutes. After completion of dropwise addition, the reaction mixture was allowed to cool to room temperature and the solvent was distilled off. The residue was purified by silica gel column chromatography [eluents: MeOH—CHCl3 (1:3) in the first run and MeOH—CHCl3 (1:10) in the second run] to give 0.23 g of the title compound as yellow crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06407248B1 |
| Source dataset | uspto-grants-2002_06 |
| ORD ID | ord-8471605050ac46ec9b29b3d11b907ee3 |
| Source note | uspto-grants-2002_06 |