HRID1667516

反应详情

EQUATION

反应方程式

HRID 1667516 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of 4-(3-bromo-phenyl)-piperazine-1-carboxylic acid tert-butyl ester (300 mg, 0.88 mmol), 2-pyrrolidin-1-yl-ethylamine (0.165 mL, 1.32 mmol), Pd2(dba)3 (40 mg, 0.044 mmol), xantphos (50 mg, 0.088 mmol) and NaOt-Bu (124 mg, 1.32 mmol) in dioxane (15 mL) was bubbled with nitrogen in a sealed tube for 10 min. The mixture was heated at 120° C. for 2 h. After this time the mixture was cooled and filtered through celite and concentrated. Chromatography on silica (ethyl acetate/MeOH) provided the title compound (203 mg, 62%). m/z (M+1) 375.53

WORKUP

后处理

  1. customwas bubbled with nitrogen in a sealed tube for 10 min
  2. temperatureAfter this time the mixture was cooled
  3. filtrationfiltered through celite and
  4. concentrationconcentrated