HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Azide → 3-Azido-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Azide | HCID 33557 | — |
| Edukt | 3-iodo-4,5-dihydro-1H-benzo[b]azepin-2(3H)-one | HCID 11033477 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 3-Azido-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one | HCID 10932520 | 83,1% |
Reaktionsschritte
To a solution of 36.7 g (128 mmol) of 3-Iodo-2,3,4,5-tetrahydro-1H-[1]-benzazapin-2-one in 200 mL of dimethylformamide was added 9.97 g (153 mmol) of sodium azide. After 3 h, the mixture was poured into 800 mL of ice water and the precipitate collected on a filter. After washing the solid successively with water, 3% aqueous sodium bisulfite, and water, the product was dried under vacuum to give 21.5 g (83%) of a tan powder. 1H NMR (300 MHz, CDCl3) d 8.91 (1H, bs), 7.4-7.0 (4H, m), 3.89 (1H, t, J=9 Hz), 2.97 (1H, m), 2.73 (1H, m), 2.52 (1H, m), 2.32 (1H, m).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05843941 |
| Quelldatensatz | uspto-grants-1998_12 |
| ORD ID | ord-75cc96b3e23e427691baa875e6e5676f |
| Quellennotiz | uspto-grants-1998_12 |