HRID1095669

反应详情

EQUATION

反应方程式

HRID 1095669 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 2,8-dibromoquinoline (22.4 g, 78.0 mmol), 7-(2-methoxyethoxy)imidazo[1,2-a]pyridine (15.0 g, 78.0 mmol), Pd(PPh3)4 (4.51 g, 3.90 mmol), K2CO3 (21.6 g, 156 mmol) and Pd(OAc)2 (0.876 g, 3.90 mmol), dioxane (312 mL) and water (3 ml) was heated to 100° C. for 18 hours. The resulting mixture was diluted with dichloromethane (500 ml) and filtered. The filtrate was concentrated under reduced pressure and to the resulting oil was added ethyl acetate (100 ml) and methyl tert-butyl ether (100 ml). The resulting mixture was stirred overnight. Filtration to collect the resulting solids yielded the title compound (22.2 g, 72% yield). MS ESI (+) m/z 398 and 400 (M+1 of each isotope) detected.

WORKUP

后处理

  1. filtrationfiltered
  2. concentrationThe filtrate was concentrated under reduced pressure and to the resulting oil
  3. additionwas added ethyl acetate (100 ml) and methyl tert-butyl ether (100 ml)
  4. filtrationFiltration
  5. customto collect the resulting solids