HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
3,5-Dichlorobenzoyl chloride → 3,5-Dichloro-N-(7,8-dimethoxy-1-phenoxy-2,3,4,5-tetrahydro-1H-3-benzazepin-3-yl)benzamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 3,5-Dichlorobenzoyl chloride | HCID 76191 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | 3-Amino-7,8-dimethoxy-1-phenoxy-2,3,4,5-tetrahydro-3-benzazepine | HCID 9818305 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 3,5-Dichloro-N-(7,8-dimethoxy-1-phenoxy-2,3,4,5-tetrahydro-1H-3-benzazepin-3-yl)benzamide | HCID 19769428 | 61,4% |
Reaktionsschritte
3,5-Dichlorobenzoyl chloride (1.7 g) was added to a solution of 3-amino-7,8-dimethoxy-1-phenoxy-2,3,4,5-tetrahydro-3-benzazepine (2.1 g) in 100 ml dichloromethane containing sodium bicarbonate (3 g). After one hour, the mixture was filtered and concentrated. The solid residue was eluted through silica with 10% ethyl acetate in dichloromethane to yield 2.4 g of light tan solid, mp 182°-184°. This solid was recrystallized from acetonitrile to yield 2 g of white crystals, mp 184°-185°.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05202319 |
| Quelldatensatz | uspto-grants-1993_04 |
| ORD ID | ord-5113fc8db5c4427cb477426f39177d1a |
| Quellennotiz | uspto-grants-1993_04 |