HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 67334316, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-Amino-4-methylpiperazine | HCID 81349 | — |
| Reactant | 4-Bromo-1-fluoro-2-nitrobenzene | HCID 2736328 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 67334316 | HCID 67334316 | 63.2% |
Reaction Steps
Heat a mixture of 1-amino-4-methyl piperazine (0.217 mol, 25.0 g), 5-bromo-2-fluoronitrobenzene (0.239 mol, 52.6 g) and triethylamine (0.46 mol, 46 g) in ethyl acetate (900 mL) to reflux for 16 h. Cool the reaction mixture to room temperature, dilute with ethyl acetate, and wash with water and brine. Dry the organic layer over anhydrous sodium sulfate, filter, and concentrate. Purify on a silica gel column using 5% methanol in dichloromethane as eluent to give the title compound (43.2 g, 63%). ES-MS m/z 315 [M+1]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07994164B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-adb7248022c14ccdae4ce44b5d4fd6fd |
| Source note | uspto-grants-2011_08 |