HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → (r)-1-(3,4,5-Trimethoxybenzoyl)-3-(2-(4-(1-methyl-1h-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-(3,4-dichlorophenyl)pyrrolidine methanesulfonic acid salt
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Isopropanol | HCID 3776 | — |
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | (R)-1-(3,4,5-trimethoxybenzoyl)-3-(2-(4-(1-methyl-1H-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-(3,4-dichlorophenyl)pyrrolidine | HCID 53998673 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | (r)-1-(3,4,5-Trimethoxybenzoyl)-3-(2-(4-(1-methyl-1h-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-(3,4-dichlorophenyl)pyrrolidine methanesulfonic acid salt | HCID 88072375 | — |
Reaction Steps
Combine (R)-1-(3,4,5-trimethoxybenzoyl)-3-(2-(4-(1-methyl-1H-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-(3,4-dichlorophenyl)pyrrolidine (0.3 g) and ethyl acetate (10 mL). Add dropwise, a solution of methanesulfonic acid (0.11 g, 1.1 mmol) in ethyl acetate (2 mL). Evaporate in vacuo to give a residue. Combine the residue and isopropanol (5 mL) and diethyl ether (200 mL). After 18 hours, a solid is obtained. Decant the supernatant and add diethyl ether. Collect the solid and dry in vacuo to give the title compound: mp; 146-160° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06211199B1 |
| Source dataset | uspto-grants-2001_04 |
| ORD ID | ord-9f2b9fa0ac114d9791d5026520f5fcc0 |
| Source note | uspto-grants-2001_04 |