HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,6-Lutidine → HCID 53638878, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,6-Lutidine | HCID 7937 | — |
| Reactant | 4-Pyridinecarboxaldehyde | HCID 13389 | — |
| Solvent | Acetic Anhydride | HCID 7918 | — |
| Product | HCID 53638878 | HCID 53638878 | — |
Reaction Steps
A solution of 2,6-dimethyl pyridine (5.8 ml, and 50 mMol), and pyridine-4-carbaldehyde (4.9 ml, and 52 mMol) in acetic anhydride (9.5 ml) is heated under reflux for 16 hours. The acetic anhydride is then evaporated in vacuo and the residue purified on column chromatography (silica gel 900 g). The column is first eluted with toluene/acetone 4:1 (5 L), then with toluene/acetone 3:1 (5 L) and finally with toluene/acetone 2:1 (15 L). The fractions containing the desired compound are combined, evaporated in vacuo. The solid residue is recrystallized from methylene chloride/diisopropyl ether and 0.956 g of white crystals are isolated. (melting point: 72-73° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06656957B1 |
| Source dataset | uspto-grants-2003_12 |
| ORD ID | ord-75209e5806e54e63a35d3a1abfcc8a51 |
| Source note | uspto-grants-2003_12 |