HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → 6-Fluoro-2-methyl-5-{4-[2-(3-nitrophenyl)ethyl]-1-piperazinyl}quinoline
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 3-Nitrophenethyl methanesulfonate | HCID 21973884 | — |
| Reactant | 6-Fluoro-2-methyl-5-(1-piperazinyl)quinoline | HCID 57444314 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 6-Fluoro-2-methyl-5-{4-[2-(3-nitrophenyl)ethyl]-1-piperazinyl}quinoline | HCID 57444315 | 42% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
N,N-Diisopropylethylamine (0.15 mL; 3 eq) was added to a solution of 2-methyl-5-(1-piperazinyl)-6-fluoro quinoline (0.075 g; 1 eq) and 2-(3-nitrophenyl)ethyl methanesulfonate (D4) (0.08; 1.1 eq) in dimethylformamide (3.0 mL). The reaction mixture was heated to 100° C. for 10 hours. The dark solution was concentrated under reduced pressure, diluted with water (3 mL) and brine (1 mL) and extracted into ethyl acetate (3×3 mL). The organic layers were combined, dried over sodium sulfate and concentrated under reduced pressure. The crude was purified by flash chromatography on silica gel, eluting with a gradient from dichloromethane to dichloromethane-methanol (98:2) affording the title compound in 42% yield (0.05 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07279481B2 |
| Source dataset | uspto-grants-2007_10 |
| ORD ID | ord-aa378e3543ce4f57b5b5eb5ce29105eb |
| Source note | uspto-grants-2007_10 |