HRID1675306

反应详情

EQUATION

反应方程式

HRID 1675306 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

A mixture of 5-bromothiophene-2-carboxaldehyde 60.1 (1.03 g, 5.4 mmol), 4-(trifluoromethyl)benzeneboronic acid 61.1 (2.05 g, 10.9 mmol), K2CO3 (2.24 g, 16.2 mmol), and Pd(PPh3)4 (0.60 g, 0.54 mmol) in toluene (15 mL) was stirred for 5 Hours at 95° C. The mixture was cooled to room temperature, filtered through a pad of silica gel (EtOAc), and concentrated. The crude product was chromatographed on silica gel (0-30% EtOAc/hexane) to afford 61.2 (0.87 g, 63%) as off-white crystals. 1H NMR (400 MHz, CDCl3) δ 9.93 (s, 1H), 7.78 (m, 3H), 7.70 (d, 2H), 7.48 (d, 1H).

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. filtrationfiltered through a pad of silica gel (EtOAc)
  3. concentrationconcentrated
  4. customThe crude product was chromatographed on silica gel (0-30% EtOAc/hexane)