HuagongsheHuagongshe Chemistry Print Report · For research reference only
Isoamyl Nitrite → HCID 86653846, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Isoamyl Nitrite | HCID 8053 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 67215914 | HCID 67215914 | — |
| Catalyst | Cupric Chloride | HCID 24014 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 86653846 | HCID 86653846 | — |
Reaction Steps
150 mg (0.287 mmol) of 2-amino-6-({[2-(4-chlorophenyl)-1,3-oxazol-4-yl]methyl}sulfanyl)-4-[3-fluoro-4-(2-hydroxyethoxy)phenyl]pyridine-3,5-dicarbonitrile (Example 20) are initially charged in 20 ml of acetonitrile, 258 μl (1.724 mmol) of isoamyl nitrite and 232 mg (1.724 mmol) of copper(II) chloride are added and the mixture is stirred at room temperature overnight. The reaction mixture is then added to saturated ammonium chloride solution and extracted with ethyl acetate. The organic phase is washed with saturated sodium chloride solution, dried over sodium sulfate and concentrated. The residue is purified by preparative HPLC (mobile phase gradient: acetonitrile/water 10:90→95:5). This gives 25 mg (16% of theory) of the target compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09095582B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-f2fde6f7f2c5490e8f44eed71d10c6ca |
| Source note | uspto-grants-2015_08 |