HRID643670

反应详情

EQUATION

反应方程式

HRID 643670 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 7-bromo-[1,2,4]triazolo[4,3-a]pyridin-3-amine (0.202 g, 0.95 mmol), N-cyclopropyl-4-methyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzamide (0.358 g, 1.2 mmol), sodium carbonate (0.439 g, 4.1 mmol) and trans-dichlorobis(triphenyl-phosphine)palladium (II) (0.057 g, 0.081 mmol) in 7 μL of DME/3 mL of H2O/2 mL of EtOH was heated at 80° C. After 2.5 h, the reaction mixture was cooled to 25° C., evaporated onto silica gel and purified by flash column chromatography eluting with 2M NH3 in MeOH:CH2Cl2 (0:1→3:97) to give the title compound as a tan amorphous solid. MS m/z: 308.1 [M+1].

WORKUP

后处理

  1. temperaturethe reaction mixture was cooled to 25° C.
  2. customevaporated onto silica gel
  3. custompurified by flash column chromatography
  4. washeluting with 2M NH3 in MeOH:CH2Cl2 (0:1→3:97)