HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hexamethyldisilazide → HCID 178507212, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| Reactant | 3-Aminopyridine-4-carbonitrile | HCID 10678219 | — |
| Reactant | HCID 178470772 | HCID 178470772 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178507212 | HCID 178507212 | — |
Reaction Steps
LiHMDS (3.0 eq) was added to ethyl 3H-imidazo[4,5-b]pyridin-2-ylacetate (1.0 eq) in THF at −78° C. After 20 minutes, a solution of 3-aminopyridine-4-carbonitrile (1.1 eq) in THF was added. The resulting mixture was allowed to warm to room temperature, stirred 3 hours, and then refluxed overnight. The mixture was cooled to 0° C. and quenched with an aqueous saturated NH4Cl solution. A precipitate formed, was filtered off, and was washed repeatedly with ether to yield the desired compound as a brown solid. Purification by reverse phase chromatography afforded the desired product as a yellow solid. LC/MS m/z 279.0 (MH+), Rt 1.29 minutes.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07138409B2 |
| Source dataset | uspto-grants-2006_11 |
| ORD ID | ord-25ac4180e596493a8a2910c52cc11210 |
| Source note | uspto-grants-2006_11 |