HuagongsheHuagongshe Chemistry Print Report · For research reference only
A-425619 → HCID 69522424, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | A-425619 | HCID 8068410 | — |
| Reactant | Potassium hydroxy sulfite | HCID 23707502 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 69522424 | HCID 69522424 | 10.5% |
Reaction Steps
To a suspension of N-isoquinolin-5-yl-N′-[4-(trifluoromethyl)benzyl]urea (Example 14; 100 mg, 0.29 mmol) in chloroform (25 ml) was added Oxone (541 mg, 0.87 mmol), followed by wet alumina Grade III (1 g), and the resulting suspension heated at reflux for 60 minutes. Whilst the mixture was still hot it was filtered to remove alumina and Oxone, the solids were washed with more chloroform, then methanol, and the filtrate evaporated to dryness. The residue was purified by preparative TLC eluting with 10% MeOH in dichloromethane+0.5% NH4OH, and the product triturated with a mixture of dichloromethane/iso-hexanes, filtered and dried to give the title compound (11 mg, 10%) as a white solid. m/z (ES+) 362 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07285563B2 |
| Source dataset | uspto-grants-2007_10 |
| ORD ID | ord-0e579f81713b4e919e4802fba7158156 |
| Source note | uspto-grants-2007_10 |