HRID711223

反应详情

EQUATION

反应方程式

HRID 711223 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
96 °C

PROCEDURE

实验过程

A mixture of 4-bromo-2-methylpyridine 13-1 (516 mg, 3.00 mmol), (4-(aminomethyl)phenyl)boronic acid hydrochloride 13-2 (422 mg, 2.25 mmol), Pd(PPh3)4 (173 mg, 0.15 mmol) and K3PO4 (1.7 g, 8 mmol) in anhydrous dioxane (10 mL) was stirred at 96° C. under argon overnight. After cooling to room temperature, the mixture was filtered through celite and washed with ethyl acetate. The filtrate was concentrated by rotavap and the residue subjected to silica gel column chromatography with 7% ammonia-saturated methanol in dichloromethane as eluent to give (4-(2-methylpyridin-4-yl)phenyl)methanamine 13-3 as an oil.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. filtrationthe mixture was filtered through celite
  3. washwashed with ethyl acetate
  4. concentrationThe filtrate was concentrated by rotavap