HRID1942622

反应详情

EQUATION

反应方程式

HRID 1942622 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

To a solution of 3-bromo-5-[4-[(1-methylethyl)oxy]-3-(trifluoromethyl)phenyl]-1,2,4-thiadiazole (D45) (487 mg), 2-{2-ethyl-3-[(E)-2-(methyloxy)ethenyl]phenyl}-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (573 mg) and tripotassium phosphate (845 mg) in N,N-dimethylformamide (DMF) (4 mL) and water (0.800 mL) stirred under nitrogen at room temp was added Pd(Ph3P)4 (153 mg). The reaction mixture was sealed and heated under microwave at 120° C. for 10 min. After cooling the reaction, the mixture was concentrated and purified by column chromatography to give 3-{2-ethyl-3-[(E)-2-(methyloxy)ethenyl]phenyl}-5-[4-[(1-methylethyl)oxy]-3-(trifluoromethyl)phenyl]-1,2,4-thiadiazole (D49) (580 mg) as a colorless oil. MS (ES): C23H23F3N2O2S requires 448. found 449.1 (M+H+).

WORKUP

后处理

  1. customThe reaction mixture was sealed
  2. temperatureAfter cooling
  3. customthe reaction
  4. concentrationthe mixture was concentrated
  5. custompurified by column chromatography