HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxybenzenesulfonic acid → 5-{8-[(3R)-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 | Ds-7423 | HCID 45378170 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 5-{8-[(3R)-4-acetyl-3-methylpiperazin-1-yl]-6-morpholin-4-yl-9-(2,2,2-trifluoroethyl)-9H-purin-2-yl}pyrimidin-2-amine benzenesulfonate | HCID 86344190 | 67% |
Reaction Steps
To a suspension of 5-{8-[(3R)-4-acetyl-3-methylpiperazin-1-yl]-6-morpholin-4-yl-9-(2,2,2-trifluoroethyl)-9H-purin-2-yl}pyrimidin-2-amine (126 mg, 0.242 mmol) in 10% aqueous ethanol solution (5 ml) was added benzenesulfonic acid mono hydrate (46.8 mg, 0.266 mmol) at 50° C., and the mixture was allowed to be cooled down to room temperature, and stirred for 15 hr. The solid precipitated out was collected and dried to give 5-{8-[(3R)-4-acetyl-3-methylpiperazin-1-yl]-6-morpholin-4-yl-9-(2,2,2-trifluoroethyl)-9H-purin-2-yl}pyrimidin-2-amine benzenesulfonate (110 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-90e0f4073cc64be590d6dd7015de62f1 |
| Source note | uspto-grants-2012_01 |