HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → (2S)-2-methyl-1-[(2-methyl-4-pyridinyl)carbonyl]-4-{[4-(trifluoromethyl)phenyl]sulfonyl}piperazine formic acid salt
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 2733084 | — |
| Edukt | 2-Methylpyridine-4-carboxylic acid | HCID 2762821 | — |
| Edukt | (S)-3-Methyl-1-((4-(trifluoromethyl)phenyl)sulfonyl)piperazine | HCID 59152086 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | (2S)-2-methyl-1-[(2-methyl-4-pyridinyl)carbonyl]-4-{[4-(trifluoromethyl)phenyl]sulfonyl}piperazine formic acid salt | HCID 44612081 | 120,7% |
Reaktionsschritte
To a solution of (3S)-3-methyl-1-{[4-(trifluoromethyl)phenyl]sulfonyl}piperazine (Description 2) (80 mg, 0.259 mmol) in DMF (5 ml) was added 2-methyl-4-pyridinecarboxylic acid (35.6 mg, 0.259 mmol), HOBT.H2O (39.7 mg, 0.259 mmol), HBTU (98 mg, 0.259 mmol) and DIPEA (0.136 ml, 0.778 mmol) and the reaction mixture was stirred at room temperature overnight. DMF was evaporated in vacuo then DCM (5 ml) was added and washed with saturated aq. NaHCO3 solution (5 ml), dried on a phase separation cartridge and evaporated in vacuo. The crude material was dissolved in MeCN/DMSO 1:1 and purified by MDAP. The desired fractions were collected and concentrated in vacuo giving the title compound (74 mg).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08530478B2 |
| Quelldatensatz | uspto-grants-2013_09 |
| ORD ID | ord-43d2502aae1d4b49bf668f12fc6946c8 |
| Quellennotiz | uspto-grants-2013_09 |