HRID1875044

反应详情

EQUATION

反应方程式

HRID 1875044 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. temperatureThe reaction mixture was cooled to room temperature
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. concentrationconcentrated