HRID1684518

反应详情

EQUATION

反应方程式

HRID 1684518 的结构方程式

CONDITIONS

反应条件

温度
23 °C

PROCEDURE

实验过程

A mixture of 2-fluoroaniline (13.0 ml), 2-fluoronitrobenzene (14.2 ml) and potassium iodide (5.5 g) was heated at 180° for 18 h. The mixture was cooled to 23° C.; the solid materials were filtered off and the solution was concentrated in vacuo. The residue was purified by flash chromatography (eluting with CH-EA 7:3) then crystallized from absolute ethanol to give the title compound as an orange solid (9.30 g). T.l.c. CH-EA (7:3), Rf =0.69. M.p. 76°-77° C. IR: 3352 (NH), 1609 (C=C), 1510 and 1350 (NO2) cm-1.

WORKUP

后处理

  1. temperaturewas heated at 180° for 18 h
  2. filtrationthe solid materials were filtered off
  3. concentrationthe solution was concentrated in vacuo
  4. customThe residue was purified by flash chromatography (eluting with CH-EA 7:3)
  5. customthen crystallized from absolute ethanol