HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,6-Dimethyl-4-nitrophenyl trifluoromethanesulfonate → 2-Bromo-1,3-dimethyl-5-nitrobenzene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,6-Dimethyl-4-nitrophenyl trifluoromethanesulfonate | HCID 22662125 | — |
| Reactant | Lithium bromide hydrate | HCID 23702478 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ammonium Chloride | HCID 25517 | — |
| Product | 2-Bromo-1,3-dimethyl-5-nitrobenzene | HCID 7022096 | 69% |
Reaction Steps
2,6-dimethyl-4-nitrophenyl trifluoromethanesulfonate (5.0 g, 17 mmol) was dissolved in N,N-dimethylformamide (40 mL). Lithium bromide monohydrate (4.7 g, 45 mmol) was added and the reaction was refluxed overnight. The reaction was diluted with saturated ammonium chloride and the layers were separated. The organics were washed with water (3×40 mL) and brine, dried over sodium sulfate, filtered and concentrated. Purification by column chromatography (2% ethyl acetate in petroleum ether) gave 2-bromo-1,3-dimethyl-5-nitrobenzene (2.7 g, 69%) as a light yellow solid. 1H NMR (400 MHz, CDCl3, δ): 7.94 (s, 2H), 2.50 (s, 6H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09056834B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-b32497e6730e4693a0d9ed0b960d9ae1 |
| Source note | uspto-grants-2015_06 |