HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloro-4-nitrobenzene → HCID 7059976, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloro-4-nitrobenzene | HCID 7443 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | rel-(2R,6S)-2,6-dimethylpiperazine | HCID 6950261 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 7059976 | HCID 7059976 | — |
Reaction Steps
1.0 g (5.21 mmol) of 3,4-dichloronitrobenzene (Fluka, Buchs, Switzerland), 624 mg (5.47 mmol) cis-2,6-dimethylpiperazine (Aldrich, Buchs, Switzerland) and 580 mg (5.73 mmol) triethylamine in 20 ml of EtOH are heated in a microwave oven at 170° C. for 6 h and 180° C. for 2 h. The reaction mixture is evaporated to dryness and then taken in EtOAc. The organic layers is extracted with 1 M aqueous HCl(5×) and the combined aqueous layers are basified with NaHCO3 and extracted with CH2Cl2 (3×), washed with brine, dried over MgSO4, filtered and evaporated to dryness to give the title compound as a yellow solid. ES-MS: 270 (M+H)+; analytical HPLC: tret=2.72 minutes (Grad 1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07667039B2 |
| Source dataset | uspto-grants-2010_02 |
| ORD ID | ord-85fd01bbcfce4e599683f804f81cd43a |
| Source note | uspto-grants-2010_02 |