HRID1875044
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 45 °C
PROCEDURE
实验过程
Trifluoroacetic acid (30 mL, 389 mmol) was added to a solution of bis(1,1-dimethylethyl) [2-fluoro-3-(1-naphthalenyloxy)-4-nitrophenyl]propanedioate (22.89, g, 46 mmol) in dichloromethane (250 mL). the mixture was heated under a reflux condenser at 45° C. for 4 hrs. The reaction mixture was cooled to room temperature and diluted with ethyl acetate and water. The organic layer was dried over sodium sulfate and concentrated to give the title compound (15.70 g, 100%). 1H NMR (400 MHz, chloroform-d) δ ppm 8.91 (br. s., 1H), 8.30-8.44 (m, 1H), 7.82-7.91 (m, 2 H), 7.51-7.62 (m, 3H), 7.21-7.35 (m, 2H), 6.58 (d, 1H), 3.82 (d, 2H). ES MS: m/z 340 (M−1).
WORKUP
后处理
- temperatureThe reaction mixture was cooled to room temperature
- dry with materialThe organic layer was dried over sodium sulfate
- concentrationconcentrated