HRID277092

反应详情

EQUATION

反应方程式

HRID 277092 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 40.5 mg (0.21 mmol) 2,6-diamino-4-bromo-pyridine, 90.5 mg (0.47 mmol) 3,4-dichloro-phenyl-boronic acid, 7.8 mg (0.01 mmol) Dichloro(1,1′-bis(diphenylphosphino) ferrocene)palladium (II) dichloromethane adduct and 0.3 ml 2M Na2CO3 in 1 ml dimethoxyethane was heated to 80° C. for 17 h. The mixture was filtered over silica washed with MeOH/DCM and concentrated. The residue was taken up in 1 ml DMF and the totle compound was purified by reversed phase column chromatography eluting wit an acetonitrile/water gradient to yield 29 mg (52%), MS m/e (%): 254 M+ (100).

WORKUP

后处理

  1. filtrationThe mixture was filtered over silica
  2. washwashed with MeOH/DCM
  3. concentrationconcentrated
  4. customthe totle compound was purified by reversed phase column chromatography
  5. washeluting wit an acetonitrile/water gradient
  6. customto yield 29 mg (52%), MS m/e (%)