HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxybenzenesulfonic acid → 5-{8-[(3S)-4-acetyl-3-methylpiperazin-1-yl]-6-morpholin-4-yl-9-(2,2,2-trifluoroethyl)-9H-purin-2-yl}pyrimidin-2-amine benzenesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxybenzenesulfonic acid | HCID 15619088 | — |
| Reactant | 5-{8-[(3S)-4-acetyl-3-methylpiperazin-1-yl]-6-morpholin-4-yl-9-(2,2,2-trifluoroethyl)-9H-purin-2-yl}pyrimidin-2-amine | HCID 45378171 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 5-{8-[(3S)-4-acetyl-3-methylpiperazin-1-yl]-6-morpholin-4-yl-9-(2,2,2-trifluoroethyl)-9H-purin-2-yl}pyrimidin-2-amine benzenesulfonate | HCID 86641994 | 77.2% |
Reaction Steps
To a suspension of 5-{8-[(3S)-4-acetyl-3-methylpiperazin-1-yl]-6-morpholin-4-yl-9-(2,2,2-trifluoroethyl)-9H-purin-2-yl}pyrimidin-2-amine (53.8 mg, 0.1 mmol) in 10% aqueous ethanol solution (0.6 ml) was added benzenesulfonic acid mono hydrate (20.0 mg, 0.11 mmol) at 50° C., and the mixture was cooled down to room temperature, and was stirred for 5 hr. The solid precipitated out was collected and dried to give 5-{8-[(3S)-4-acetyl-3-methylpiperazin-1-yl]-6-morpholin-4-yl-9-(2,2,2-trifluoroethyl)-9H-purin-2-yl}pyrimidin-2-amine benzenesulfonate (52.4 mg) as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08097622B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-81f3988dae1642a6b5ffbcdff7bc7a34 |
| Source note | uspto-grants-2012_01 |