HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Lithium Chloride → N-Trifluoroacetyl-7-(2-Methyl-2H-pyrazol-3-yl)-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Lithium Chloride | HCID 433294 | — |
| Edukt | 1-Methyl-5-(tributylstannyl)-1H-pyrazole | HCID 21867455 | — |
| Edukt | N-Trifluoroacetyl-7-hydroxy-1-methyl-2,3,4,5-tetrahydro-1H-3benzazepine | HCID 22292790 | — |
| Katalysator | HCID 178418476 | HCID 178418476 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | N-Trifluoroacetyl-7-(2-Methyl-2H-pyrazol-3-yl)-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine | HCID 22292810 | — |
Reaktionsschritte
To a solution of N-trifluoroacetyl-7-hydroxy-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine, O-trifluoromethanesulfonate (100 mg, 0.25 mmol) in dimethylformamide (2 mL) was treated with (2-methyl-2H-pyrazol-3-yl)-tri-n-butyltin (138 mg, 0.37 mmol), LiCl (21 mg, 0.50 mmol), Pd(PPh3)2Cl2 (35 mg, 0.05 mmol) and stirred at 100 C for 4 hours. The product mixture was diluted with EtOAc (20 mL), washed twice with water (10 mL), once with brine (10 mL), dried with Na2SO4 and concentrated. Flash chromatography (30% EtOAc in hexane, silica) resulted in 80 mg of a clear oil. MS calculated for C17H18F3N3O+H: 338, observed: 338.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08846906B2 |
| Quelldatensatz | uspto-grants-2014_09 |
| ORD ID | ord-eda1b82965154befa98e6e2f5d37116f |
| Quellennotiz | uspto-grants-2014_09 |