HRID524039

反应详情

EQUATION

反应方程式

HRID 524039 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A mixture of 6-bromopyrido[2,3-d]pyrimidin-2-amine (1.0 g, 4.46 mmol), 3,5-dimethoxyphenylboronic acid (1.2 g, 6.70 mmol), PdCl2(dppf) (364 mg, 0.446 mmol) and potassium carbonate (1.8 g, 13.39 mmol) in 1,4-dioxane/water (4 mL/1 mL) was degassed with nitrogen for 5 min and stirred at 110° C. for 30 min under microwave. The reaction mixture was cooled to RT, and concentrated to afford a crude product, which was purified by silica gel column chromatography (ethyl acetate:petroleum ether=4:1) to afford 6-(3,5-dimethoxyphenyl)pyrido[2,3-d]pyrimidin-2-amine as a yellow solid (400 mg, 31%). MS (ES+) C15H14N4O2 requires: 282. found: 283 [M+H]+.

WORKUP

后处理

  1. customwas degassed with nitrogen for 5 min
  2. temperatureThe reaction mixture was cooled to RT
  3. concentrationconcentrated
  4. customto afford a crude product, which
  5. customwas purified by silica gel column chromatography (ethyl acetate:petroleum ether=4:1)