Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Nitric Acid | HCID 944 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Benzene, 2,4-dichloro-1-(methylsulfonyl)- | HCID 158897 | — |
| Product | HCID 21876463 | HCID 21876463 | 74% |
Reaction Steps
A mixture of (2,4-dichloro-phenyl)-methyl sulfone (Ono Mitsunori, Nakamura Yoshisada, Sato Shingo, Itoh Isamu, Chem. Lett, 1988, 395–398.; 3.33 g, 16 mmol) and sulfuric acid (conc, 14 ml) was added a mixture of sulfuric acid (4 ml) and nitric acid (fuming, 2 ml) dropwise under ice-water bath. The mixture was stirred at 55° C. for 1 h. The mixture was poured onto ice-water and neutralized with 6N aqueous NaOH and then extracted with dichloromethane. The organic layer was washed with brine and dried (Na2SO4). The solvent was removed under reduced pressure and the residue was purified by flash chromatography eluting with hexane/ethyl acetate (2:1/1:1) to give 3 g (74%) of the title compound as white solids.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07141580B2 |
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| Source dataset | uspto-grants-2006_11 |
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| ORD ID | ord-875ef03aa93b42bfaf47f2eeb13f03bc |
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| Source note | uspto-grants-2006_11 |
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