HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → 4-(2-Amino-4-nitro-phenylsulfanyl)-phenol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 2-Chloro-5-nitroaniline | HCID 22691 | — |
| Reactant | 4-Mercaptophenol | HCID 240147 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 4-(2-Amino-4-nitro-phenylsulfanyl)-phenol | HCID 66808421 | 46% |
Reaction Steps
A solution of 2-Chloro-5-nitroaniline (3 g, 17.4 mmole), 4-hydroxythiophenol (2.4 g, 19.0 mmol), cesium carbonate (12.35 g, 38 mmol) in dimethylformamide (35 ml) was heated at 100° C. for 16 hours. Afterwards ice water (200 mL) was added to the solution and to the resultant slurry was added ethyl acetate (200 ml). The layers were separated and the organic layer was washed with 10% sodium bicarbonate and 10% sodium chloride, dried over anhydrous sodium sulfate. The drying agent was filtered and solvent was removed under vacuum leaving a yellow oil. The oil was purified by silica gel chromatography eluting with methylene chloride/methanol (97:3), to provide a yellow solid as the title compound (2.1 g, 46%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07915411B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-464b8c0f0d594079837483b259aecc5c |
| Source note | uspto-grants-2011_03 |