HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → 1-(2,6-Dichlorophenyl)piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 2,6-Dichloro-N-phenylaniline | HCID 84867 | — |
| Reactant | Bis(2-chloroethyl)amine hydrochloride | HCID 522769 | — |
| Product | 1-(2,6-Dichlorophenyl)piperazine | HCID 11492345 | — |
Reaction Steps
A mixture of 2,6-dichlorophenylaniline (810 mg, 5 mmol, Aldrich) and bis(2-chloroethyl)amine hydrochloride (823 mg, 5 mmol, Aldrich) was subjected to microwave irradiation at 200° C. for 10 min. The reaction mixture was allowed to cool to room temperature then treated with 5N NaOH (5 mL) and extracted with EtOAc (2×20 mL). The combined organic extracts were washed with brine (5 mL), dried over Na2SO4 and filtered. The solvent was removed in vacuo and the residue was purified by silica gel chromatography, eluting with 10% MeOH/CH2Cl2+1% ammonia (30% in water) to give the title compound. MS (ESI, pos. ion) m/z: 231 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08026241B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-7739c52eccd04b9bb90ee009de2421c2 |
| Source note | uspto-grants-2011_09 |