HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 178428440, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | Sodium Nitrite | HCID 23668193 | — |
| Reactant | HCID 67141952 | HCID 67141952 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178428440 | HCID 178428440 | 33.4% |
Reaction Steps
Sodium azide (137 mg, 2.1 mmol) was added at 0° C. to a solution of 1-(3-chlorobenzyl)-7-(3,4-dihydro-1H-isoquinolin-2-yl)-2,3-dimethyl-1H-pyrrolo[2,3-c]pyridin-5-carbonitrile (300 mg, 0.7 mmol) prepared in Example 689 and ammonium chloride (74.9 mg, 1.4 mmol) in anhydrous N,N-dimethylformamide (10 ml). The reaction mixture was refluxed overnight. 6% sodium nitrite solution was added to the reaction mixture, which was then extracted with ethyl acetate. The organic layer was dried on anhydrous magnesium sulfate and then concentrated under reduced pressure. The resulting residue was purified with silica gel column chromatography (ethyl acetate/n-hexane=1/3, v/v) to give 110 mg of the titled compound as a white solid. (Yield: 33%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07662832B2 |
| Source dataset | uspto-grants-2010_02 |
| ORD ID | ord-4bab9a874c6244608e273c98ce175992 |
| Source note | uspto-grants-2010_02 |