HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 67112088, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Phosphoric Acid | HCID 1004 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | tert-butyl 4-(4-ethyl-1-(2-(pyrrolidin-1-yl)ethyl)-1H-imidazol-2-yl)piperidine-1-carboxylate | HCID 67954430 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67112088 | HCID 67112088 | 72% |
Reaction Steps
Combine tert-butyl 4-(4-ethyl-1-(2-(pyrrolidin-1-yl)ethyl)-1H-imidazol-2-yl)piperidine-1-carboxylate; phosphoric acid (18.27 g, 38.50 mmol) and water (9.1 mL). Add 12 M hydrochloric acid in water (9.63 mL, 3.0 eq) dropwise and stir at room temperature. After one hour, adjust the pH of the reaction mixture with 2 M aqueous sodium hydroxide to 10. Dilute with dichloromethane. Separate the layers. Wash the aqueous phase with dichloromethane. Wash the organics with aqueous saturated sodium chloride. Dry the organics over anhydrous magnesium sulfate, filter, and concentrate in vacuo to give 4-(4-ethyl-1-(2-(pyrrolidin-1-yl)ethyl)-1H-imidazol-2-yl)piperidine (7.70 g, 72%). MS (ES) m/z=277 [M]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08436002B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-7100c854b7c94b55b5a3587da813d4b7 |
| Source note | uspto-grants-2013_05 |