2,3,4-trifluoroaniline

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 7.70 g of sodium borohydride was added to a mixture of 3.70 g of 2,3,4-trifluoroaniline, 10.30 g of sodium acetate, 20 ml of acetone, 19.6 ml of acetic acid and 39 ml of water under stirring and ice-cooling. After 2 hours, the reaction mixture was made alkaline with sodium carbonate and extracted with benzene. The extract was washed with NaCl saturated water, dried and the solvent was evaporated to give 3.17 g of 2,3,4-trifluoro-N-isopropyl aniline as colorless oil. ice-cooling extracted with benzene The extract was washed with NaCl saturated water dried the solvent was evaporated

反応条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 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. the suspension obtained is filtered the filtrate is concentrated under reduced pressure (20 kPa) at a temperature in the region of 50° C 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 concentrated under reduced pressure (20 kPa) at approximately 30° C