HRID1256186

反应详情

EQUATION

反应方程式

HRID 1256186 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

Under argon atmosphere, 200 mg (892 μmol, 1 eq) of 7-bromo-1,5-naphthyridin-2-ylamine, 196.3 mg (1.07 mmol, 1.2 eq) of 3,4,5-trimethoxyaniline, 2 mg (2.3 μmol, 0.0025 eq) tris(dibenzylideneacetone)dipalladium, 4 mg (6.7 μmol, 0.0075 eq) 2,2′-bis(diphenylphosphino)-1,1′-binaphtyl and 120 mg (1.24 mmol, 1.4 eq) of sodium terbutoxide were introduced in 6 mL of toluene. The mixture was stirred at 80° C. for 24 h. The mixture was allowed to reach it and water was added. Aqueous layer was extracted with methylene chloride. Organic layers were dried over Na2SO4, filtered and evaporated to dryness. The residue was purified by column chromatography using methylene chloride/ethanol: 96/4 as eluent. The solvent was evaporated to dryness to afford 50 mg of yellow powder with 17% yield.

WORKUP

后处理

  1. additionwas added
  2. extractionAqueous layer was extracted with methylene chloride
  3. dry with materialOrganic layers were dried over Na2SO4
  4. filtrationfiltered
  5. customevaporated to dryness
  6. customThe residue was purified by column chromatography
  7. customThe solvent was evaporated to dryness