HRID1627253

反应详情

EQUATION

反应方程式

HRID 1627253 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
56 °C

PROCEDURE

实验过程

A mixture of 5-(2-(3,4-dichlorophenyl)propan-2-yl)-1-(4-fluorophenyl)-1H-imidazole-2(3H)-thione (760 mg, 2 mmol), 4-(bromomethyl)-3,5-difluorobenzonitrile (464 mg, 2 mmol) and K2CO3 (414 mg, 3 mmol) in acetone (10 mL) was stirred at 56° C. for 4 h. After cooling, the solids were removed by filtration and rinsed with acetone. The combined filtrates were concentrated and purified by flash chromatography, eluting with EtOAc-Hexane (1:1) to afford the title compound (89 mg). 1H NMR (400 MHz, CDCl3) δ 7.26 (t, J=4.2, 2H), 7.17 (d, J=6.5, 2H), 7.03 (d, J=2.2, 1H), 6.88-6.79 (m, 3H), 6.50-6.44 (m, 2H), 4.08 (d, J=9.1, 2H), 2.04 (s, 1H), 1.49 (s, 7H); MS (EI) m/z 432 (MH+).

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe solids were removed by filtration
  3. washrinsed with acetone
  4. concentrationThe combined filtrates were concentrated
  5. custompurified by flash chromatography
  6. washeluting with EtOAc-Hexane (1:1)