HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → t-Butyl 4-(3-(1-(3,5-dimethylphenyl)ethylamino)-4-nitrophenyl)piperazine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| Reactant | 5-fluoro-N-(1-(3,5-dimethylphenyl)ethyl)-2-nitrobenzenamine | HCID 58707336 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | t-Butyl 4-(3-(1-(3,5-dimethylphenyl)ethylamino)-4-nitrophenyl)piperazine-1-carboxylate | HCID 58707281 | 43% |
Reaction Steps
5-fluoro-N-(1-(3,5-dimethylphenyl)ethyl)-2-nitrobenzenamine (762 mg, 2.4 mmol), t-butyl piperazine-1-carboxylate (443 mg, 2.4 mmol), N,N-diisopropylethylamine (614 mg, 4.8 mmol) were stirred at 80° C. in dry acetonitrile (50 mL) for 48 h. The solvent was evaporated and the residue was dissolved in dichloromethane and washed with water. The dichloromethane was evaporated and the crude compound was purified by silica chromatography using 25% ethyl acetate in hexanes to afford the title compound (469 mg, 41% yield). 1H NMR (400 MHz, CDCl3): δ 8.68 (s, 1H), 8.05 (d, 1H), 6.49 (s, 2H), 6.33 (s, 1H), 6.14 (d, 1H), 5.70 (s, 1H), 4.47 (m, 1H), 3.76 (s, 6H), 3.43 (m, 4H), 3.23 (m, 2H), 3.15 (m, 2H), 1.62 (d, 3H), 1.46 (s, 9H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07968538B2 |
| Source dataset | uspto-grants-2011_06 |
| ORD ID | ord-e54bc23cd34d43b1adb8ff3102fca521 |
| Source note | uspto-grants-2011_06 |