HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Trimethylaluminum → HCID 178489759, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Trimethylaluminum | HCID 16682925 | — |
| Edukt | Ethyl ether methylene chloride | HCID 21881112 | — |
| Edukt | Ethyl 4-(4-cyclopropyl-1,4-diazepan-1-yl)benzoate | HCID 66589916 | — |
| Edukt | HCID 178489815 | HCID 178489815 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | HCID 178489759 | HCID 178489759 | 33,7% |
Reaktionsschritte
4-(4-cyclopropyl-1,4-diazepan-1-yl)-N-[5-[2-(3,5-dimethoxyphenyl)ethyl]-2H-pyrazol-3-yl]benzamide was prepared using the same procedure as for Example 159, but starting from ethyl 4-(4-cyclopropyl-1,4-diazepan-1-yl)benzoate (0.288 g, 1 mmol, 5-[2-(3,5-dimethoxyphenyl)ethyl]-2H-pyrazol-3-amine (0.247 g, 1 mmol) and a 2M solution of trimethylaluminium (1.250 mL, 2.50 mmol) in toluene. The crude product 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 a gum which solidified on trituration with DCM/Ether to afford the title compound (0.165 g, 33.7%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07737149B2 |
| Quelldatensatz | uspto-grants-2010_06 |
| ORD ID | ord-82fab6006a0a4d4182d2a06c28df6589 |
| Quellennotiz | uspto-grants-2010_06 |