HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 178482247, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | 2-Chloro-6-[4-(methylamino)piperidin-1-yl]isonicotinonitrile | HCID 86038383 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178482247 | HCID 178482247 | 37.1% |
Reaction Conditions
| Temperature | 120 °C |
|---|
Reaction Steps
Sodium azide (131 mg, 2.02 mmol) and NH4Cl (108 mg, 2.02 mmol) were added to a solution of 2-chloro-6-[4-(methylamino)piperidin-1-yl]isonicotinonitrile (Intermediate 63, 507 mg, 2.02 mmol) in anhydrous DMF (3 ml). The mixture was heated at 120° C. under nitrogen gas for 1 h where LCMS showed the expected mass. The mixture was filtered and was purified by semi-preparative HPLC eluting with acetonitrile/water (0.1% TFA) and the title compound was concentrated in vacuo to give a hygroscopic brown solid (220 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07709503B2 |
| Source dataset | uspto-grants-2010_05 |
| ORD ID | ord-08f0d26f503747cc989ca118c020fe52 |
| Source note | uspto-grants-2010_05 |