HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic 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 methanesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | Ds-7423 | HCID 45378170 | — |
| Solvent | Dichloromethane methanol | HCID 21226129 | — |
| 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 methanesulfonate | HCID 54755937 | 96.5% |
Reaction Steps
To a solution 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 (100.4 mg, 0.18 mmol) in methanol/dichloromethane solution (2/3, 3.5 ml) was added methanesulfonic acid (11.9 μl, 0.18 mmol) at room temperature, and the mixture was stirred for 10 minutes. Then the solvent was removed in reduced pressure, and the resultant solid was 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 methanesulfonate (107.1 mg) as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08309546B2 |
| Source dataset | uspto-grants-2012_11 |
| ORD ID | ord-542913931aea469a9c35b3bc61595691 |
| Source note | uspto-grants-2012_11 |