Reaktion #337646

Reaktionsgleichung

Potassium carbonate

5-nitro-isoindole-1,3-dione

bromo-acetic acid ethyl ester

→

title compound

(5-Nitro-1,3-dioxo-1,3-dihydro-isoindol-2-yl)-acetic acid ethyl ester

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe resulting mixture was refluxed overnight (18 h)
2. 2
   TemperaturAfter cooling
3. 3
   Sonstigereaction mixture
4. 4
   Filtrationwas filtered
5. 5
   Waschenrinsed with ethyl acetate
6. 6
   EinengenFiltrate was concentrated
7. 7
   Sonstigethe residue was triturated with ether (200 ml)
8. 8
   SonstigeSolid was collected
9. 9
   Waschenrinsed with ether
10. 10
    SonstigeDried in vacuo

Vorschrift

Potassium carbonate (57.8 g) was added to a solution mixture of 5-nitro-isoindole-1,3-dione (26.2 g) and bromo-acetic acid ethyl ester (25.1 g) in actone (500 ml). The resulting mixture was refluxed overnight (18 h). After cooling, reaction mixture was filtered and rinsed with ethyl acetate. Filtrate was concentrated and the residue was triturated with ether (200 ml). Solid was collected and rinsed with ether. Dried in vacuo to give the title compound 231.9 g. 1H NMR (200 MHz, CDCl3) δ 8.69 (m, 2H), 8.07 (d, J=8.2 Hz, 1H), 4.48 (s, 2H), 4.24 (q, J=7.0 Hz, 2H), 1.30 (t, J=7.0 Hz, 3H).

Quelle