HRID472161

反应详情

EQUATION

反应方程式

HRID 472161 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

4-fluoronitrobenzene (32.3 g; 0.229 mol) and 4-methyl-1H-imidazole (25 g; 0.3 mol) are mixed at r.t., to this stirred mixture K2CO3 (44 g; 0.3 mol) is added. The reaction mixture is then heated at 120° C. overnight, then cooled at r.t. and poured in water (2 L), the resulting suspension is filtered and washed with water. The obtained solid is dried at 60° C. and recrystallized from ethyl acetate (600 mL), to provide the title compound as a yellow solid (22.5 g; 48.3%). The regioisomer, 4-(5-methyl-1H-imidazol-1yl)nitrobenzene remains in the crystallization mother liquor along with a certain amount of the titled product (TLC: hexane/AcOEt 3:2). C10H9N3O2, MW 203.2.

WORKUP

后处理

  1. additionis added
  2. temperaturecooled at r.t.
  3. filtrationthe resulting suspension is filtered
  4. washwashed with water
  5. customThe obtained solid is dried at 60° C.
  6. customrecrystallized from ethyl acetate (600 mL)