HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxybenzenesulfonic acid → HCID 86641962, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxybenzenesulfonic acid | HCID 15619088 | — |
| Reactant | 2-(5-amino-4,6-dimethylpyrimidine-2-yloxy)-N-(1-benzylpiperidine-4-yl)-N-methylacetamide | HCID 25099089 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 86641962 | HCID 86641962 | 75.7% |
Reaction Steps
Compound 65 (200 mg) was suspended in methanol (1 mL) and benzenesulfonic acid monohydrate (83.4 mg) was added to the suspension at room temperature (20 to 30° C.). After the compound was dissolved, the mixture was concentrated under reduced pressure. Then, isopropanol (2.0 mL) was added to the resulting residue and the mixture was stirred under reflux. Water (230 μL) was then added portionwise. Once the residue was dissolved, the mixture was stirred overnight as it was allowed to cool. Subsequently, the mixture was stirred and cooled with ice for 1 hour, and was suction-filtered. The resulting solid was washed with isopropanol and dried to give 194 mg (69% yield) of the desired product as white crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08685989B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-1604116e78b24a5585bb4ceaa13ec7cd |
| Source note | uspto-grants-2014_04 |