HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Acetone → 1-Ethyl-7-(3-iodopropoxy)-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Acetone | HCID 180 | — |
| Edukt | Sodium Iodide | HCID 5238 | — |
| Edukt | 7-(3-Chloropropoxy)-1-ethyl-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione | HCID 68673253 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 1-Ethyl-7-(3-iodopropoxy)-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione | HCID 68672792 | 99,7% |
Reaktionsschritte
7-(3-Chloropropoxy)-1-ethyl-3,3,5-trimethyl-1,5-dihydro-benzo[b][1,4]diazepine-2,4-dione (2.18 g) and sodium iodide (4.8 g) were added to acetone (50 ml), and heated under reflux for 8.5 hours. The reaction mixture was cooled to room temperature, water was added, and extraction with ethyl acetate was performed. The organic layer was dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=1:1). The purified product was concentrated under reduced pressure to give the title compound(2.76 g) as a colorless oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09212187B2 |
| Quelldatensatz | uspto-grants-2015_12 |
| ORD ID | ord-c5e6b820dd8341c0a5ad0d36777e9b1a |
| Quellennotiz | uspto-grants-2015_12 |