反应详情

温度

120 °C

2-(2-Nitro-4-trifluoromethylphenyl)-malonic acid dimethyl ester (68 g, 0.21 mol) was dissolved in dimethyl sulfoxide (200 mL). Sodium chloride (34 g, 0.58 mol) and water (60 mL) were added and the mixture was stirred for 16-20 h at 120° C. (reaction monitored by TLC). The reaction mixture was then cooled to room temperature and quenched into water, which caused precipitation of the product. After stirring for 30 minutes, the product. (45 g, 80%) was isolated by filtration. The product was used without further purification in the next reaction. A small sample was crystallized (EtOAc/hexane, 2:8) for analysis, to yield yellow crystals, mp 104-105° C. 1H NMR (CDCl3) 8.3 (s, 1H), 7.88 (d, J=8.4 Hz, 1H), 7.50 (d, J=8.4 Hz, 1H), 4.12 (s, 2H), 3.60 (s, 3H). MS (FAB) m/z: 275.2 (M++1).

1. custom(reaction monitored by TLC)
2. temperatureThe reaction mixture was then cooled to room temperature
3. customquenched into water, which
4. customprecipitation of the product
5. stirringAfter stirring for 30 minutes
6. custom(45 g, 80%) was isolated by filtration
7. customThe product was used without further purification in the next reaction
8. customA small sample was crystallized (EtOAc/hexane, 2:8) for analysis
9. customto yield yellow crystals, mp 104-105° C