HuagongsheHuagongshe Chemistry Print Report · For research reference only
rel-(2R,6S)-2,6-dimethylpiperazine → HCID 178489798, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | rel-(2R,6S)-2,6-dimethylpiperazine | HCID 6950261 | — |
| Reactant | HCID 178489782 | HCID 178489782 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 178489798 | HCID 178489798 | 35.2% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
(2S,6R)-2,6-Dimethylpiperazine (228 mg, 2.00 mmol) was added in one portion to 5-chloro-N-[5-[2-(3,5-dimethoxyphenyl)ethyl]-2H-pyrazol-3-yl]pyrazine-2-carboxamide (388 mg, 1.00 mmol) in anhydrous dimethylsulfoxide (1.00 ml) at 25° C. The resulting solution was stirred at 100° C. for 18 h. The crude product was purified by ion exchange chromatography, using an SCX column. The desired product was eluted from the column using 7M NH3/MeOH to afford impure material. The concentrated eluent was purified by preparative HPLC, using decreasingly polar mixtures of water (containing 1% NH3) and MeCN as eluents. Fractions containing the desired compound were evaporated to dryness to afford the title compound (164 mg, 35%) as a cream solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07737149B2 |
| Source dataset | uspto-grants-2010_06 |
| ORD ID | ord-f3403cefc69c4b158649f4ab3d6f009a |
| Source note | uspto-grants-2010_06 |