HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → 1-(3,4,5-Trimethoxybenzoyl)-3-(2-(4-(1-(2-methylsulfonylethyl)-1h-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-(3,4-difluorophenyl) pyrrolidine methanesulfonic acid salt
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 9853348 | HCID 9853348 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | 1-(3,4,5-Trimethoxybenzoyl)-3-(2-(4-(1-(2-methylsulfonylethyl)-1h-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-(3,4-difluorophenyl) pyrrolidine methanesulfonic acid salt | HCID 22009176 | — |
Reaction Steps
Combine 1-(3,4,5-trimethoxybenzoyl)-3-(2-(4-(1-(2-methylsulfonylethyl)-1H-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-(3,4-difluorophenyl) pyrrolidine (1.0 g, 1.38 mmol) and ethyl acetate (50 mL). Add methanesulfonic acid (0.27 g, 2.76 mmol). Heat to reflux. After 1 hour, cool to ambient temperature and stir. After 40 hours, add diethyl ether (150 mL) to give a solid. Repeatedly, decant the solvent add diethyl ether before collecting the solid and drying in vacuo to give the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06211199B1 |
| Source dataset | uspto-grants-2001_04 |
| ORD ID | ord-a474e043dcc4479ab42d4422e919f057 |
| Source note | uspto-grants-2001_04 |