HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 22716473, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 1,2-Difluoro-4-nitrobenzene | HCID 123053 | — |
| Reactant | HCID 22716476 | HCID 22716476 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 22716473 | HCID 22716473 | 72.4% |
Reaction Steps
1-(2-Fluoroethyl)-2-oxopiperazine trifluoroacetate (6.1 g) was dissolved in acetonitrile (100 ml). N,N-Diisopropylethylamine (13 ml) was added to the mixture, followed by 3,4-difluoronitrobenzene (3.39 g), and the mixture heated to reflux for 18 hours. Solvent was evaporated, and the residue chromatographed on silica, using as eluant a gradient increasing in polarity from 0 to 4% methanol in dichloromethane. Relevant fractions were combined and evaporated to give 3-fluoro-4-(4-{2-fluoroethyl}-3-oxopiperazin-1-yl)nitrobenzene product as a solid (4.4 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06069145 |
| Source dataset | uspto-grants-2000_05 |
| ORD ID | ord-c746c89f0b9c494896dd3c2d7cc8d7bc |
| Source note | uspto-grants-2000_05 |