反応 #2254162

反応方程式

potassium carbonate

2-iodopropane

N,N-dimethylformamide

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

→

3-amino-3-hydroxyimino-2-isopropoxyiminopropionitrile

収率 53.9%

溶媒

water

反応条件

後処理

1. 1
   抽出followed by extraction with ethyl acetate
2. 2
   その他The organic layer obtained
3. 3
   洗浄was washed with a saturated aqueous sodium chloride solution
4. 4
   乾燥dried over anhydrous magnesium sulfate
5. 5
   ろ過filtered
6. 6
   その他to remove inorganic matter
7. 7
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
8. 8
   その他The resulting residue was purified by silica gel column chromatography (ethyl acetete:hexane=1:2)

実験手順

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).

出典