HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 6-(hydroxymethyl)-2-(4-(methylsulfonyl)phenyl)-5-(piperidin-4-yloxy)pyridazin-3(2H)-one HCl salt
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | Tert-butyl 4-(3-(hydroxymethyl)-1-(4-(methylsulfonyl)phenyl)-6-oxo-1,6-dihydropyridazin-4-yloxy)piperidine-1-carboxylate | HCID 67072635 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 6-(hydroxymethyl)-2-(4-(methylsulfonyl)phenyl)-5-(piperidin-4-yloxy)pyridazin-3(2H)-one HCl salt | HCID 67072611 | 100% |
Reaction Steps
To a stirring solution of tert-butyl 4-(3-(hydroxymethyl)-1-(4-(methylsulfonyl)phenyl)-6-oxo-1,6-dihydropyridazin-4-yloxy)piperidine-1-carboxylate (200 mg, 0.417 mmol) in DCM (3 mL) at room temperature under argon was added 4 M HCl in dioxane (0.521 mL, 2.085 mmol). The reaction mixture was stirred at room temperature overnight. Et2O (10 mL) was added to the reaction mixture. The solid product was collected by filtration and further washed with ether (2 mL×2). After drying under vacuum for 2 hours, 171 mg (100%) of 6-(hydroxymethyl)-2-(4-(methylsulfonyl)phenyl)-5-(piperidin-4-yloxy)pyridazin-3(2H)-one HCl salt was obtained as an off-white solid. MS (ESI) 380 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08372837B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-d6067dd9c16848b68c47710a0d614b32 |
| Source note | uspto-grants-2013_02 |