HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine, 2,4,6-trichloro- → HCID 59617901, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine, 2,4,6-trichloro- | HCID 27665 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 3-Cyclopropyl-3-fluoroazetidine hydrochloride | HCID 66589642 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 59617901 | HCID 59617901 | 36.4% |
Reaction Steps
A solution of 2,4,6-trichloropyridine (3.0 g, 16.4 mmol), 3-cyclopropyl-3-fluoroazetidine hydrogen chloride (2.49 g, 16.4 mmol) and DIPEA (7.09 ml, 41.0 mmol) in ethanol (40 ml) was heated under reflux for 1 h. Reaction mixture cooled to room temperature then concentrated to dryness in vacuo. Crude product purified by flash chromatography on silica (0 to 100% EtOAc:petrol) to give title compound as a white solid (1.56 g, 36%). 1H NMR (CDCl3) 0.52-0.48 (2H, m), 0.72-0.67 (2H, m), 1.42-1.31 (1H, m), 3.91 (2H, ddd), 4.05 (2H, ddd), 6.20 (2H, s). ES+ 261.30.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08785444B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-3150b942e2d044fe91ddfd2a6b777951 |
| Source note | uspto-grants-2014_07 |