HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 89813171, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | HCID 89812849 | HCID 89812849 | — |
| Reactant | HCID 178418260 | HCID 178418260 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 89813171 | HCID 89813171 | 77.5% |
Reaction Steps
A mixture of 7-(2-Ethyl-phenoxy)-4-hydroxy-1-iodo-isoquinoline-3-carboxylic acid methyl ester (1.5 g, 3.34 mmole) and copper cyanide (598 ml, 6.68 mmole) in anhydrous dimethylformamide (13 ml) was refluxed for 5 minutes before it was cooled to room temperature and dichloromethane was added and stirred for 5 minutes. The suspension was filtered. The filtrate was washed with 0.1 N HCl, twice with water, brine, dried over anhydrous sodium sulfate and concentrated in vacuo. The residue was recrystallized with acetonitrile. The crystal was filtered and dried to give the title compound as a white solid (902 mg): MS: (+) m/z 349.08 (M+1), (−) m/z 347.10 (M−1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09409892B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-b5347073dc7745ceb801b3e66e80e51a |
| Source note | uspto-grants-2016_08 |