HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Aminopyridine → HCID 18348915, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Aminopyridine | HCID 1727 | — |
| Reactant | O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate | HCID 2733207 | — |
| Reactant | HCID 18348865 | HCID 18348865 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 18348915 | HCID 18348915 | 61.1% |
Reaction Steps
2-(3-Formyl-5-methyl-phenoxy)-acetic acid (0.47 g) and 4-aminopyridine (0.46 g) were dissolved in dry DMF (10 ml). The resulting solution, stirring under a nitrogen atmosphere, was treated with TBTU (0.82 g). The resulting mixture was stirred for 68 h and then concentrated at reduced pressure to give a yellow viscous gum. This crude material was purified by preparative hplc. The purified product was partitioned between ethyl acetate and an aqueous solution saturated with sodium bicarbonate, sodium chloride and ammonium sulphate. The organic phase was dried over magnesium sulphate and concentrated under reduced pressure giving the title compound as an off-white solid (0.40 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06326386B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-e9e6181139d44d588c6528e4ede37b65 |
| Source note | uspto-grants-2001_12 |