HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 21192427, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 21192453 | HCID 21192453 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 21192427 | HCID 21192427 | 71.4% |
Reaction Steps
POCl3 (46 μL, 0.50 mmol) was added to a stirred suspension of 4-chloro-7-(phenylsulfanyl)-1-(2H)-isoquinolone (120 mg, 0.42 mmol) in MeCN (2 mL) at 23° C., and the mixture was heated at reflux for 1.5 h which gave a clear solution. This cooled solution was poured into water (20 mL) and the mixture was extracted with EtOAc (×3). The combined organic extracts were washed with brine, dried (Na2SO4) and evaporated in vacuo. The residue was purified by column chromatography upon silica gel using hexanes-EtOAc (90:10) as eluant to give 1,4-dichloro-7-(phenylsulfanyl)isoquinoline (92 mg, 0.30 mmol) as an oil which solidified on standing.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06248738B1 |
| Source dataset | uspto-grants-2001_06 |
| ORD ID | ord-94b0b0b3a9c8464da9b2355e398849a7 |
| Source note | uspto-grants-2001_06 |