HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 12074220, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Piperazine | HCID 4837 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 378891 | HCID 378891 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 12074220 | HCID 12074220 | 53.4% |
Reaction Steps
To a mixture of piperazine (1.0 g, 12 mmol) and potassium carbonate (2.0 g, 14 mmol) in 80 mL of dry acetonitrile is added 4-fluoro-2-nitro-1-(phenylsulfanyl) benzene (2, EXAMPLE 1, step 1, 2.7 g, 9.5 mmol). The mixture is allowed to stir overnight at rt. Water and CH2Cl2 (80 mL each) are added and the layers separated. The aqueous layer is extracted with CH2Cl2 (3×50 mL). The combined organic layers are dried over MgSO4, filtered, and concentrated. Purification via column chromatography (50% EtOAc/hexane) gives 1.6 g (47%) of the title compound as a red oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06586592B2 |
| Source dataset | uspto-grants-2003_07 |
| ORD ID | ord-6e639b94569d4ecb8c0d2b1769377300 |
| Source note | uspto-grants-2003_07 |