反应详情

温度

20 °C

2,3,4-Trifluoroaniline (58.8 g) is added in a single portion with stirring to a solution of 2-ethoxycarbonyl-1-ethoxyethylideneamine hydrochloride (90 g) in ethanol (820 cc). After 48 hours' stirring at a temperature in the region of 20° C., the suspension obtained is filtered; the filtrate is concentrated under reduced pressure (20 kPa) at a temperature in the region of 50° C. The oily residue is taken up with water (250 cc). The mixture obtained is extracted with ethyl ether (3×200 cc). The combined organic extracts are washed with water (4×150 cc), dried over magnesium sulphate and concentrated under reduced pressure (20 kPa) at approximately 30° C. 2,3,4-Trifluoro-N-[1-ethoxy-2-(ethoxycarbonyl)ethylidene]aniline (122 g) is obtained in the form of a yellow oil, which is used without further purification for the subsequent steps.

1. customthe suspension obtained
2. filtrationis filtered
3. concentrationthe filtrate is concentrated under reduced pressure (20 kPa) at a temperature in the region of 50° C
4. customThe mixture obtained
5. extractionis extracted with ethyl ether (3×200 cc)
6. washThe combined organic extracts are washed with water (4×150 cc)
7. dry with materialdried over magnesium sulphate
8. concentrationconcentrated under reduced pressure (20 kPa) at approximately 30° C