HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ammonium Hydroxide → 6-bromo-8-methoxy-4,4-dimethyl-1,4-dihydro-2H-3,1-benzoxazin-2-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ammonium Hydroxide | HCID 14923 | — |
| Edukt | Bromine | HCID 24408 | — |
| Edukt | 2H-3,1-Benzoxazin-2-one, 1,4-dihydro-4,4-dimethyl-8-methoxy- | HCID 210617 | — |
| Edukt | Sodium Acetate | HCID 517045 | — |
| Lösungsmittel | Acetic Acid | HCID 176 | — |
| Produkt | 6-bromo-8-methoxy-4,4-dimethyl-1,4-dihydro-2H-3,1-benzoxazin-2-one | HCID 23509642 | 93,4% |
Reaktionsschritte
To a mixture of 8-methoxy-4,4-dimethyl-1,4-dihydro-2H-3,1-benzoxazin-2-one (2.1 g, 10.1 mmol), sodium acetate (1.5 g, 18 mmol) in acetic acid (30 mL) was added bromine (0.62 mL, 12 mmol) at ambient temperature. After 30 minutes, the solution was treated with a concentrated ammonium hydroxide solution (50 mL). The precipitate was collected on a filter and washed with water (3×20 mL) to yield 6-bromo-8-methoxy-4,4-dimethyl-1,4-dihydro-2H-3,1-benzoxazin-2-one (2.7 g, 93%) as off-white solid: MS (ESI) m/z 286, 288 [M+H]+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06713478B2 |
| Quelldatensatz | uspto-grants-2004_03 |
| ORD ID | ord-57356ea393df435c9d4c129165c98866 |
| Quellennotiz | uspto-grants-2004_03 |