HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethyl bromoacetate → 7-Bromo-2H-(1,4)-benzothiazin-3(4h)-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethyl bromoacetate | HCID 7748 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | 2-Amino-5-bromobenzene-1-thiol | HCID 1209045 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 7-Bromo-2H-(1,4)-benzothiazin-3(4h)-one | HCID 689065 | 82% |
Reaktionsschritte
A mixture of 2-amino-5-bromo-benzenethiol (20 g, 0.1 mol), ethyl bromoacetate (19 g, 0.1 mol), and sodium bicarbonate (8.8 g, 0.1 mol) in DMF (200 ml) was heated to reflux for 2 hours. The mixture was diluted with water and extracted with ethyl acetate (2×100 mL). The combined organic extracts were washed with water, then brine, dried (MgSO4) and evaporated to obtain the crude 7-bromo-4H-benzo[1,4]thiazin-3-one (20 g, 82%). A small portion of sample was recrystallized from ethanol to afford pure 7-bromo-4H-benzo[1,4]thiazin-3-one: mp 212-213° C.; MS (EI) m/z 243/245 (M+).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06794373B2 |
| Quelldatensatz | uspto-grants-2004_09 |
| ORD ID | ord-e50172ae9f6142a88197f249cfba527d |
| Quellennotiz | uspto-grants-2004_09 |