Реакция #2254162

Уравнение реакции

potassium carbonate

2-iodopropane

N,N-dimethylformamide

3-amino-2,3-bis(hydroxyimino)propionitrile

→

3-amino-3-hydroxyimino-2-isopropoxyiminopropionitrile

Выход 53.9%

Растворители

water

Условия реакции

Обработка

1. 1
   Экстракцияfollowed by extraction with ethyl acetate
2. 2
   ДругоеThe organic layer obtained
3. 3
   Промывкаwas washed with a saturated aqueous sodium chloride solution
4. 4
   Сушкаdried over anhydrous magnesium sulfate
5. 5
   Фильтрацияfiltered
6. 6
   Другоеto remove inorganic matter
7. 7
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
8. 8
   ДругоеThe resulting residue was purified by silica gel column chromatography (ethyl acetete:hexane=1:2)

Методика

2.52 g (14.8 mM) of 2-iodopropane was added to an N,N-dimethylformamide solution (30 ml) of 2.00 g (15.6 mM) of 3-amino-2,3-bis(hydroxyimino)propionitrile. The mixture was cooled to 0° C. 2.05 g (14.8 mM) of potassium carbonate was added, followed by stirring at room temperature for 16 hours. The reaction mixture was poured into water, followed by extraction with ethyl acetate. The organic layer obtained was washed with a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and filtered to remove inorganic matter. The solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography (ethyl acetete:hexane=1:2) to obtain 1.36 g (yield: 51%) of 3-amino-3-hydroxyimino-2-isopropoxyiminopropionitrile (compound No. 1-004).

Источник