HRID1942589

反应详情

EQUATION

反应方程式

HRID 1942589 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

To a suspension of 2-bromo-5-{3-chloro-4-[(1-methylethyl)oxy]phenyl}-1,3,4-thiadiazole (D10) (0.5 g), 2-ethyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzaldehyde (D5) (0.468 g) and tripotassium phosphate (0.795 g) in N,N-dimethylformamide (DMF) (10 mL) and Pd(Ph3P)4 (0.173 g). The reaction mixture was degassed and then the reaction vial was sealed and heated under microwave at 130° C. for 10 min. Water was then added to the reaction mixture. The mixture was extracted with EA. The combined organic solution was dried over anhydrous sodium sulphate. After filtration and concentration, the residue was purified by column chromatography to give 3-(5-{3-chloro-4-[(1-methylethyl)oxy]phenyl}-1,3,4-thiadiazol-2-yl)-2-ethylbenzaldehyde (D11) (164 mg). MS (ES): C20H19ClN2O2S requires 386. found 387.1 (M+H+).

WORKUP

后处理

  1. customThe reaction mixture was degassed
  2. customthe reaction
  3. customvial was sealed
  4. extractionThe mixture was extracted with EA
  5. dry with materialThe combined organic solution was dried over anhydrous sodium sulphate
  6. filtrationAfter filtration and concentration
  7. customthe residue was purified by column chromatography