HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Chloro-3-nitrobenzenesulfonamide → HCID 22730653, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Chloro-3-nitrobenzenesulfonamide | HCID 7324 | — |
| Reactant | Benzenamine, 2-phenoxy- | HCID 75899 | — |
| Reactant | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 22730653 | HCID 22730653 | — |
Reaction Steps
A −78° C. solution of Example 1C (236 mg, 1.0 mmol) and 2-phenoxyaniline (370 mg, 2.0 mmol) in THF (10 mL) was treated with 1M lithium hexamethyldisilazide in THF (4 mL, 4.0 mmol), warmed to room temperature over 4 hours, diluted with ethyl acetate (50 mL), washed sequentially with 1M HCl (5 mL), water (5 mL), and brine (5 mL), dried (MgSO4), filtered, and concentrated. The concentrate was purified by flash column chromatography on silica gel with 10-30% ethyl acetate/hexanes to provide the desired product. MS (ESI(−)) m/e 384 (M−H)−.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07754886B2 |
| Source dataset | uspto-grants-2010_07 |
| ORD ID | ord-6d24b1d4a574468480c3ed8e6e8bded3 |
| Source note | uspto-grants-2010_07 |