HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hexamethyldisilazide → HCID 178461496, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| Reactant | 2-amino-6-[(2R,6S)-2,6-dimethylmorpholin-4-yl]benzonitrile | HCID 68668486 | — |
| Reactant | HCID 178470772 | HCID 178470772 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178461496 | HCID 178461496 | — |
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 2-amino-6-[(2R,6S)-2,6-dimethylmorpholin-4-yl]benzonitrile (1.1 eq) in THF was added. The resulting mixture was allowed to warm to room temperature, stirred for 2 hours and then heated to 60° C. overnight. The mixture was cooled to 0° C. and quenched with an aqueous saturated NH4Cl solution. The aqueous phase was extracted with CH2Cl2 (5 times) and the organic extracts were collected, dried (Na2SO4), and concentrated. The crude product was purified by HPLC. LC/MS m/z 391.2 (MH+), Rt 2.35 minutes.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06800760B2 |
| Source dataset | uspto-grants-2004_10 |
| ORD ID | ord-fa95680e770a41cd825852282b362c27 |
| Source note | uspto-grants-2004_10 |