HRID884639

反应详情

EQUATION

反应方程式

HRID 884639 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

In a pressure vessel was added methyl 4-bromo-2-methylbenzoate (500 mg, 2.18 mmol), Dioxane (5.0 mL), Cs2CO3 (1.4 g, 4.36 mmol), and Xantphos (92.0 mg, 0.16 mmol). The mixture was stirred and nitrogen was bubbled into the reaction for 5 min before adding in Palladium(II) acetate (58 mg, 0.08 mmol), and commercially available N-methyl piperazine (0.26 mL, 2.62 mmol). The vessel was then sealed and heated to 100° C. overnight. The reaction was cooled and filtered through celite. The supernatant was then concentrated and column purified (5:95 EtOAc:Hexanes) to give methyl 2-methyl-4-(4-methylpiperazin-1-yl)benzoate (480 mg, 89% yield).

WORKUP

后处理

  1. customnitrogen was bubbled into the reaction for 5 min
  2. customThe vessel was then sealed
  3. temperatureThe reaction was cooled
  4. filtrationfiltered through celite
  5. concentrationThe supernatant was then concentrated
  6. customcolumn purified (5:95 EtOAc:Hexanes)