HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → 1-(3,4,5-Trimethoxybenzyl)-3-(3-(4-(1-(2-ethoxyethyl)-1h-benzimidazol-2-yl-amino)piperidin-1-yl)propyl)-3-(4-fluorophenylmethyl)-2-oxopyrrolidine methanesulfonic acid salt
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 1-(3,4,5-trimethoxybenzyl)-3-(3-(4-(1-(2-ethoxyethyl)-1H-benzimidazol-2-yl-amino)piperidin-1-yl)propyl)-3-(4-fluorophenylmethyl)-2-oxopyrrolidine | HCID 9918134 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | 1-(3,4,5-Trimethoxybenzyl)-3-(3-(4-(1-(2-ethoxyethyl)-1h-benzimidazol-2-yl-amino)piperidin-1-yl)propyl)-3-(4-fluorophenylmethyl)-2-oxopyrrolidine methanesulfonic acid salt | HCID 22009303 | — |
Reaction Steps
Combine 1-(3,4,5-trimethoxybenzyl)-3-(3-(4-(1-(2-ethoxyethyl)-1H-benzimidazol-2-yl-amino)piperidin-1-yl)propyl)-3-(4-fluorophenylmethyl)-2-oxopyrrolidine (0.91 g, 1.28 mmol) and ethyl acetate (15 mL). Add methanesulfonic acid (0.25 g, 2.57 mmol) and heat to reflux. After 1 hour, cool to ambient temperature and stir. After 12 hours, add diethyl ether and decant the solvent. Repeatedly, add diethyl ether and decant to give a solid. Collect the solid by filtration and dry in vacuo to give the title compound. Rf=0.24 (silica gel, 10% methanol/ethyl acetate/2% triethylamine).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06211199B1 |
| Source dataset | uspto-grants-2001_04 |
| ORD ID | ord-9f7aacea7c134c27ad7c2ae971a3b45b |
| Source note | uspto-grants-2001_04 |