HRID1942633

反应详情

EQUATION

反应方程式

HRID 1942633 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

To a solution of 5-(3-bromo-1,2,4-thiadiazol-5-yl)-2-(2-methylpropyl)benzonitrile (D60) (500 mg), 2-{2-ethyl-3-[(E)-2-(methyloxy)ethenyl]phenyl}-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (470 mg) and tripotassium phosphate (988 mg) in N,N-dimethylformamide (DMF) (6 mL) and water (1.5 mL) stirred under nitrogen was added Pd(Ph3P)4 (179 mg). The mixture was sealed and heated under microwave at 120° C. for 15 min. After cooling the reaction, the mixture was diluted with ethyl acetate, washed with water, dried over sodium sulphate, concentrated and purified by column chromatography to give 5-(3-{2-ethyl-3-[(E)-2-(methyloxy)ethenyl]phenyl}-1,2,4-thiadiazol-5-yl)-2-(2-methylpropyl)benzonitrile (D61) (500 mg). MS (ES): C24H25N3OS requires 403. found 404.2 (M+H+).

WORKUP

后处理

  1. customThe mixture was sealed
  2. temperatureAfter cooling
  3. customthe reaction
  4. washwashed with water
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated
  7. custompurified by column chromatography