تفاعل #2254162

معادلة التفاعل

potassium carbonate

2-iodopropane

N,N-dimethylformamide

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

→

3-amino-3-hydroxyimino-2-isopropoxyiminopropionitrile

المردود 53.9%

المذيبات

water

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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).

المصدر