HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 178516764, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | HCID 23506248 | HCID 23506248 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178516764 | HCID 178516764 | 31.8% |
Reaction Conditions
| Temperature | 130 °C |
|---|
Reaction Steps
2-(3-Cyanophenoxy)-3-[3-(3-hydroxypyridin-4-yl)propoxy]-pyridine (0.85 g, 2.5 mmol) obtained in Example 28 is dissolved in DMF (10 ml), and thereto are added sodium azide (0.20 g, 3.0 mmol) and ammonium chloride (0.16 g, 3.0 mmol). The mixture is stirred at 130° C. for one hour, and the reaction solution is concentrated under reduced pressure. The residue thus obtained is purified by silica gel column chromatography (eluent: acetic acid/ethanol), and recrystallized from ethanol to give the title compound (0.31 g) as pale brown crystals, m.p. 220-240° C. (decomposed).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06765095B2 |
| Source dataset | uspto-grants-2004_07 |
| ORD ID | ord-6b3c0dbd45c24ce89617683663444c9a |
| Source note | uspto-grants-2004_07 |