HuagongsheHuagongshe Chemistry Print Report · For research reference only
Toluene → HCID 117899776, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Hexane | HCID 8058 | — |
| Reactant | Methyl morpholine oxide | HCID 82029 | — |
| Reactant | HCID 123296293 | HCID 123296293 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 117899776 | HCID 117899776 | 76.3% |
Reaction Steps
To 200 ml of toluene were added 20.24 g (58.5 mmol) of [2,4-dimethyl-5-(2,2,2-trifluoroethylthio)phenyl]-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (a compound described in PCT International Publication No. WO 2012/176856 as Compound No. 55-47) and 8.22 g (70.16 mmol) of N-methylmorpholine-N-oxide. The mixture was refluxed for 2 hours under heating. The reaction mixture was allowed to cool to room temperature, washed and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography (developing solvent: a mixed solvent of n-hexane:ethyl acetate=20:1), to obtain 10.54 g (yield: 76%) of an intended product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09332754B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-6ffb426d1ddf47a2b143e9a79d506b7b |
| Source note | uspto-grants-2016_05 |