HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic 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 methanesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| 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 | Dichloromethane methanol | HCID 21226129 | — |
| 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 methanesulfonate | HCID 54756051 | 84.9% |
Reaction Steps
To a solution 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 (33.2 mg, 0.06 mmol) in methanol/dichloromethane solution (1/1, 1 ml) was added methanesulfonic acid (3.9 μl, 0.06 mmol) at room temperature, and the mixture was stirred for 3 hr. Then the solvent was removed in reduced pressure, and the resultant solid was 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 methanesulfonate (31.4 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-93a651dee8bb4bc997d04da028b35864 |
| Source note | uspto-grants-2012_01 |