HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 1-(3,4,5-Trimethoxybenzoyl)-3-(2-(4-(1-(2-ethoxyethyl)-1h-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-(3,4-dichlorophenyl)pyrrolidine methanesulfonic acid salt
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | 1-(3,4,5-trimethoxybenzoyl)-3-(2-(4-(1-(2-ethoxyethyl)-1H-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-(3,4-dichlorophenyl)pyrrolidine | HCID 9940131 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 1-(3,4,5-Trimethoxybenzoyl)-3-(2-(4-(1-(2-ethoxyethyl)-1h-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-(3,4-dichlorophenyl)pyrrolidine methanesulfonic acid salt | HCID 22009195 | — |
Reaction Steps
Combine 1-(3,4,5-trimethoxybenzoyl)-3-(2-(4-(1-(2-ethoxyethyl)-1H-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-(3,4-dichlorophenyl)pyrrolidine (0.31 g, 0.42 mmol) and ethyl acetate (15 mL). Add a solution of methanesulfonic acid (0.11 g, 1.15 mmol) in ethyl acetate (2 mL). After 18 hours evaporate in vacuo to give a residue. Combine the residue and methanol (10 mL). Add diethyl ether (190 mL) to form a solid. Collect the solid and dry in vacuo at 82° C. to give the title compound: mp; 130-135° C. (shrink, dec).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06211199B1 |
| Source dataset | uspto-grants-2001_04 |
| ORD ID | ord-ee458129988246d6be45587420ea09a0 |
| Source note | uspto-grants-2001_04 |