HRID1470354

反应详情

EQUATION

反应方程式

HRID 1470354 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

To a 10 mL sealed tube with stirbar was added 7-chloro-2-phenylfuro[3,2-b]pyridine (50.00 mg; 0.22 mmol; 1.00 eq.), 6-aminoindazole (34.79 mg; 0.26 mmol; 1.20 eq.), palladium(II) acetate (2.44 mg; 0.01 mmol; 0.05 eq.), 2-(dicyclohexylphosphino)-2′,4′,6′-triisopropylbiphenyl (10.38 mg; 0.02 mmol; 0.10 eq.), and sodium tert. butoxide (62.77 mg; 0.65 mmol; 3.00 eq.). The reagents were suspended in dioxane (2.00 ml) under a N2 atmosphere and stirred at 110° C. overnight. The reaction mixture was cooled to room temperature and concentrated on a rotary evaporator. The crude mixture was purified by Biotage chromatography (0-10% MeOH/CH2Cl2, 30 column vol) to afford the title compound as a brown solid (6.6 mg, 9%). (HPLC (method F): 97%, RT: 3.97 min); MS (m/z) 327 [M+H]+, RT: 2.6 min.

WORKUP

后处理

  1. customTo a 10 mL sealed tube with stirbar
  2. temperatureThe reaction mixture was cooled to room temperature
  3. concentrationconcentrated on a rotary evaporator
  4. customThe crude mixture was purified by Biotage chromatography (0-10% MeOH/CH2Cl2, 30 column vol)