Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Piperazine | HCID 4837 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 58707278 | HCID 58707278 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 58707258 | HCID 58707258 | 63.8% |
Reaction Steps
A solution of N-(5-fluoro-2-(methylsulfonyl)phenyl)chroman-4-amine (0.3 g, 0.93 mmol), piperazine (0.80 g, 9.33 mmol) and N,N-diisopropylethylamine (2.2 mL, 12.74 mmol) in acetonitrile (15 mL) was stirred at reflux for 16 h. The reaction mixture was cooled down and concentrated under reduced pressure. The residue was taken up in dichloromethane, washed with water, dried and concentrated in vacuo to yield 0.23 g of the crude aniline. The crude product was purified by PTLC (20% ethyl acetate in hexanes) to yield 144 mg (40%) of N-(2-(methylsulfonyl)-5-(piperazin-1-yl)phenyl)chroman-4-amine: 1H NMR (400 MHz, CD3Cl): δ 7.63 (d, 1H), 7.31 (d, 1H), 7.28 (m, 1H), 6.91 (m, 1H), 6.85 (d, 1H), 6.47 (d, 1H), 6.42 (d, 1H), 6.21 (s, 1H), 4.80 (br s, 2H), 4.65 (m, 1H), 4.23 (m, 2H), 3.04 (m, 4H), 2.88 (s, 3H), 2.21 (m, 2H), 2.20 (br d, 1H). MS (ESI) m/z: Calculated: 387.16; Observed: 388.2 (M++1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08604021B2 |
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| Source dataset | uspto-grants-2013_12 |
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| ORD ID | ord-279eb243ea034970b726a35fe143da88 |
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| Source note | uspto-grants-2013_12 |
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