HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → 2-(1-Benzothien-2-yl)-5-[(2-bromobutanoyl)amino]benzamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 2-Bromobutanoyl bromide | HCID 117293 | — |
| Edukt | 5-Amino-2-(1-benzothien-2-yl)benzamide | HCID 59428475 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 2-(1-Benzothien-2-yl)-5-[(2-bromobutanoyl)amino]benzamide | HCID 59428488 | — |
Reaktionsschritte
5-Amino-2-(1-benzothien-2-yl)benzamide (Example 8A, 886 mg) and triethylamine (650 mg) are introduced into DCM (20 ml) at 0° C., and 2-bromobutyryl bromide (1000 mg) is slowly added. The reaction mixture is warmed to RT and then stirred overnight. The reaction mixture is subsequently diluted with DCM (100 ml) and washed with 5% strength potassium bisulfate solution (twice 50 ml), dried (sodium sulfate) and concentrated in a rotary evaporator. The residue is chromatographed on silica gel (eluent cyclohexane-ethyl acetate 10:1 to 1:1). After concentration of the relevant fraction, 607 mg (47% of theory) of product are isolated.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07776922B2 |
| Quelldatensatz | uspto-grants-2010_08 |
| ORD ID | ord-5de46038a5c34b34aec8ba454fa68e3f |
| Quellennotiz | uspto-grants-2010_08 |