HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyrrolidine → 5-Fluoro-2-(3-pyrrolidin-1-ylmethyl-benzo[d]isoxazol-6-yloxy)-benzonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyrrolidine | HCID 31268 | — |
| Reactant | 2-(3-Bromomethylbenzo[d]isoxazol-6-yloxy)-5-fluorobenzonitrile | HCID 67409267 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 5-Fluoro-2-(3-pyrrolidin-1-ylmethyl-benzo[d]isoxazol-6-yloxy)-benzonitrile | HCID 67410170 | 94% |
Reaction Steps
2-(3-Bromomethylbenzo[d]isoxazol-6-yloxy)-5-fluorobenzonitrile (4v) (0.295 g, 0.850 mmol) was dissolved in dichloromethane and pyrrolidine was added dropwise (0.18 g, 2.5 mmol). After 2 hours, the reaction was concentrated and partitioned between NaHCO3 (15 mL) and EtOAc (30 mL). The aqueous layer was back extracted with EtOAc and the organic fractions were combined, washed with brine and dried (MgSO4) to provide compound (5v) (0.27 g, 94%) which was used without further purification. 1H NMR (400 MHz, CDCl3) δ 7.90 (d, J=8.6 Hz, 1H), 7.42 (d, J=6.3 Hz, 1H), 7.30-7.26 (m, 1H), 7.11 (s, 1H), 7.07-7.02 (m, 2H), 4.02 (s, 2H), 2.62 (s, 4H), 1.82 (s, 4H); MS (ESI+) m/z 338 (M+H) detected.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08518983B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-cb3330c575fb4d0a959d95f669f791c9 |
| Source note | uspto-grants-2013_08 |