Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Imidazole | HCID 795 | — |
| Reactant | Potassium Phosphate, Tribasic | HCID 62657 | — |
| Reactant | HCID 57418360 | HCID 57418360 | — |
| Catalyst | [(1R,2R)-Cyclohexane-1,2-diyl]dimethanamine | HCID 22812115 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 24906239 | HCID 24906239 | 75% |
Reaction Steps
A suspension of (R)-1-(3-bromophenylsulfonyl)-4-(4-fluoro-2-(trifluoromethyl)phenyl)-2-methylpiperazine (168 mg, 0.35 mmol), 1,2-trans-diaminomethylcyclohexane (2.9 mg, 0.015 mmol), K3PO4 (8.5 mmg, 0.06 mmol) and Imidazole (41 mg, 0.6 mmol) in dioxane (0.6 mL) was degassed and heated to 120° C. in a sealed tube till disappearance of starting material as monitored by LCMS. The crude reaction mixture was filtered through a pad of Celite and washed with EtOAc. The crude product was purified on SiO2 column eluted with hexanes/EtOAc to give the desired product as a white solid (123 mg, 75%). HRMS: calcd for C21H20F4N4O2S+H+, 469.13158. found (ESI-FTMS, [M+H]1+), 469.13336.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07632838B2 |
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| Source dataset | uspto-grants-2009_12 |
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| ORD ID | ord-9382926982d843d3a56d666ec4c36883 |
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| Source note | uspto-grants-2009_12 |
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