HRID1599081

反应详情

EQUATION

反应方程式

HRID 1599081 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 1-fluoro-2-nitrobenzene (7.47 mL, 70.9 mmol) in ethanol (35 mL) and H2O (105 mL) was added 4-amino-1,3,5-trimethylpyrazole (8.8 g, 70.9 mmol). The solution was refluxed for 15 h, then cooled to room temperature. The precipate was separated by filteration and washed with 25% aqueous ethanol to yield the title compound (8.6 g): 1HNMR (CDCl3, 300 MHz) δ 8.81 (s, 1H), 8.18 (dd, 2H, J=1.6, 8.7), 6.69(m, 1H) 6.61 (dd, 1H, J=1.2, 8.7), 3.77 (s, 3H), 2.10 (s, 3H), 2.06 (s, 3H); low resolution MS(FAB) m/z 247(MH+).

WORKUP

后处理

  1. temperatureThe solution was refluxed for 15 h
  2. customThe precipate was separated by filteration
  3. washwashed with 25% aqueous ethanol