HRID1684518
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperaturewas heated at 180° for 18 h
- filtrationthe solid materials were filtered off
- concentrationthe solution was concentrated in vacuo
- customThe residue was purified by flash chromatography (eluting with CH-EA 7:3)
- customthen crystallized from absolute ethanol