HRID250464
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
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).
WORKUP
后处理
- temperatureThe resulting mixture was refluxed overnight (18 h)
- temperatureAfter cooling
- customreaction mixture
- filtrationwas filtered
- washrinsed with ethyl acetate
- concentrationFiltrate was concentrated
- customthe residue was triturated with ether (200 ml)
- customSolid was collected
- washrinsed with ether
- customDried in vacuo