HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 68467974, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Piperidine, 1-(2-chloroethyl)-, hydrochloride | HCID 74826 | — |
| Reactant | HCID 59299341 | HCID 59299341 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | HCID 68467974 | HCID 68467974 | 196.5% |
Reaction Steps
Charge a vial with 3-(3-chloro-4′-hydroxy-biphenyl-4-ylmethyl)-1-cyclohexyl-pyrrolidin-2-one (70 mg, 0.18 mmol) and dissolve in acetone (0.3 M). Add K2CO3 (250 mg, 1.8 mmol) and Cs2CO3 (59 mg, 0.18 mmol) and stir at room temperature for 5 minutes. Add 1-(2-chloro-ethyl)-piperidine hydrochloride (77 mg, 0.42 mmol) and heat to 50° C. overnight. Cool to room temperature, filter, concentrate and purify over silica gel. Dissolve the residue in methylene chloride (0.1 M) and add 2 M HCl in ether (0.18 mL, 0.36 mmol) and concentrate in vacuo to afford 94 mg (97%) of the title compound: Mass spectrum (apci) m/z=495.4 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07713979B2 |
| Source dataset | uspto-grants-2010_05 |
| ORD ID | ord-f912cd4ed1954a51ba9b455109915d85 |
| Source note | uspto-grants-2010_05 |