HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Methylpiperazine → HCID 135444737, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Reactant | Tris(1,1-dimethylethyl)phosphine | HCID 83681 | — |
| Reactant | Sodium t-butoxide | HCID 23676156 | — |
| Reactant | HCID 136005920 | HCID 136005920 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 135444737 | HCID 135444737 | 85% |
Reaction Steps
In a stream of argon, 207 μl (1.87 mmol) of N-methylpiperazine, 120 mg (1.25 mmol) of sodium tert-butoxide, 12.6 mg (0.062 mmol) of tri-tert-butylphosphine, and 7.0 mg (0.031 mmol) of palladium(II) acetate were added to an 8 ml toluene solution of 260 mg (0.623 mmol) of the compound obtained in Example 26, and the mixture was heated under reflux for 5 hours. Then, the reaction mixture was brought to room temperature, diluted with water, and then extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate, and then the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (chloroform/methanol=20/1) to obtain 230 mg (85%) of the captioned compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07268128B2 |
| Source dataset | uspto-grants-2007_09 |
| ORD ID | ord-84b2acaf0f9a4d02a35a3e475aad9af9 |
| Source note | uspto-grants-2007_09 |