HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-(5-Chloro-2-nitrophenyl)-4-methylpiperazine → 1-{5-Chloro-2-nitro-3-{[(4-fluorophenyl)sulfonyl]methyl}phenyl}-4-methylpiperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-(5-Chloro-2-nitrophenyl)-4-methylpiperazine | HCID 2829618 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Reactant | 1-Chloromethanesulfonyl-4-fluoro-benzene | HCID 58904791 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1-{5-Chloro-2-nitro-3-{[(4-fluorophenyl)sulfonyl]methyl}phenyl}-4-methylpiperazine | HCID 44242966 | — |
Reaction Steps
A stirred mixture of 1-(5-chloro-2-nitrophenyl)-4-methylpiperazine (1.0 mmol) and chloromethyl-(4-fluorophenyl)sulfone (1.0 mmol) in THF is treated with 2.2 mL of a 1M KOt-Bu (2.2 mmol) solution in THF at −78° C., warmed to room temperature over a 2 h period, quenched with acetic acid and concentrated in vacuo. The resultant residue is partitioned between EtOAc and aqueous Na2CO3. The phases are separated and the aqueous phase is extracted with EtOAc. The organic phase is combined with the extracts, dried over Na2SO4 and concentrated to dryness in vacuo to afford the title product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07560470B2 |
| Source dataset | uspto-grants-2009_07 |
| ORD ID | ord-3eadec08c29a4541ab6365f82af9c31a |
| Source note | uspto-grants-2009_07 |