Реакция #157990

Уравнение реакции

2-(Difluoromethoxy)aniline

1,2-dibromo-1,1,2,3,3,3-hexafluoropropane

sodium hydrogen carbonate

sodium dithionite

→

1-(1-bromo-1,1,2,3,3,3-hexafluoropropan-2-yl)-6-(difluoromethoxy)aniline

Выход 26.0%

Растворители

tert-butylmethyl ether

water

Условия реакции

Обработка

1. 1
   ЭкстракцияThe reaction solution was extracted twice with ethyl acetate
2. 2
   Промывкаwashed with water
3. 3
   Сушкаdried over anhydrous magnesium sulfate
4. 4
   ФильтрацияThe drying agent was filtered off
5. 5
   Другоеthe solvent was removed by distillation under the reduced pressure
6. 6
   ДругоеThe resulting residues were purified by column chromatography

Методика

2-(Difluoromethoxy)aniline (1280 mg) and 1,2-dibromo-1,1,2,3,3,3-hexafluoropropane (8610 mg) were dissolved in tert-butylmethyl ether (30 ml) and water (30 ml), and added with tetrabutylammonium hydrogen sulfate salt (270 mg), sodium hydrogen carbonate (2030 mg) and sodium dithionite (4200 mg) in order. The mixture was stirred vigorously at room temperature for 2 days. The reaction solution was extracted twice with ethyl acetate. The organic phases were combined and washed with water, and dried over anhydrous magnesium sulfate. The drying agent was filtered off and the solvent was removed by distillation under the reduced pressure. The resulting residues were purified by column chromatography to obtain 1-(1-bromo-1,1,2,3,3,3-hexafluoropropan-2-yl)-6-(difluoromethoxy)aniline (810 mg, 26%).

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