HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → (3-Bromo-2-methylphenyl)(methyl)sulfane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 2-Bromo-6-fluorotoluene | HCID 2736335 | — |
| Reactant | Sodium methanethiolate | HCID 4378561 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | (3-Bromo-2-methylphenyl)(methyl)sulfane | HCID 57448061 | 57.8% |
Reaction Conditions
| Temperature | 150 °C |
|---|
Reaction Steps
To a solution of 1-bromo-3-fluoro-2-methylbenzene (2.0 g, 10.6 mmol) in N,N-dimethylformamide (10 ml) was added sodium methanethiolate (0.85 g, 11.7 mmol) and the mixture was stirred for 15 min at 150° C. After cooling, aqueous sodium carbonate (10%, 50 ml) was added and the phases were separated. The aqueous phase was extracted with ethylacetate (2×50 ml) and the combined organic phases was dried (MgSO4) and evaporated under reduced pressure to give an oil. The residue was purified by flash column chromatography (isooctane) to give the title compound (1.33 g). MS m/z (relative intensity, 70 eV) 218 (M+, 98), 216 (M+, 92), 202 (26), 200 (26), 122 (bp), 121 (56).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08314126B2 |
| Source dataset | uspto-grants-2012_11 |
| ORD ID | ord-515d9902fee94efd929005b5645a6f84 |
| Source note | uspto-grants-2012_11 |