HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → HCID 69433632, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 2,5-Dichloropyridine | HCID 27685 | — |
| Reactant | HCID 22940604 | HCID 22940604 | — |
| Solvent | Isoamyl Alcohol | HCID 31260 | — |
| Product | HCID 69433632 | HCID 69433632 | 65.1% |
Reaction Steps
A mixture of 1.35 g (5.56 mmol) of (7R,9aS)-7-hydroxymethyl-2,3,4,6,7,8,9,9a-octahydro-1H-pyrido[1,2-a]pyrazine dihyrochloride (Preparation 1), 4.11 g (27.8 mmol) of 2,5-dichloropyridine, 2.94 g (27.8 mmol) of sodium carbonate and 60 mL of isoamyl alcohol was heated at reflux for 48 h. The mixture was cooled and the solvent removed in vacuo. Purification by flash silica gel chromatography with 95:5 chloroform: methanol gave 1.02 g (65%) of the title compound. mp (base) 139.0-140.5° C. 13C NMR (CDCl3): δ26.8, 29.1, 39.1, 45.3, 50.8, 54.6, 58.6, 60.6, 66.2, 107.7, 120.1, 137.1,146.2, 157.6.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06231833B1 |
| Source dataset | uspto-grants-2001_05 |
| ORD ID | ord-ed67d73456c44aaa914fc89218212eff |
| Source note | uspto-grants-2001_05 |