반응 #2254164

반응 방정식

potassium carbonate

hydrogen peroxide

sodium thiosulfate

3-amino-3-hydroxyimino-2-isopropoxyiminopropionitrile

( 1 )

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

hydrogen peroxide

→

title compound

수율 63.0%

3-amino-3-hydroxyimino-2-isopropoxyiminopropanamide

수율 63.0%

용매

dimethyl sulfoxide

methanol

반응 조건

후처리

1. 1
   workup.ADDITIONwere added, at room temperature
2. 2
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
3. 3
   workup.ADDITIONWater was added to the residue and extraction with ethyl acetate
4. 4
   세척The organic layer was washed with a saturated aqueous sodium chloride solution
5. 5
   건조dried over anhydrous magnesium sulfate
6. 6
   여과filtered
7. 7
   기타to remove inorganic matter
8. 8
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
9. 9
   세척The resulting crude crystal was washed with a 1:2 mixed solution of diisopropyl ether and n-hexane

실험 절차

To a mixed solution of methanol (1.5 ml) and dimethyl sulfoxide (0.5 ml), of 0.50 g (2.94 mM) of the 3-amino-3-hydroxyimino-2-isopropoxyiminopropionitrile obtained in (1) of Example 1 were added, at room temperature, 0.73 g (6.4 mM) of a 30% aqueous hydrogen peroxide solution and 0.02 g (0.14 mM) of potassium carbonate. Stirring was conducted at room temperature for 4 hours. Excessive hydrogen peroxide was treated with an aqueous sodium thiosulfate solution. The solvent was distilled off under reduced pressure. Water was added to the residue and extraction with ethyl acetate was conducted. The organic layer 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 crude crystal was washed with a 1:2 mixed solution of diisopropyl ether and n-hexane to obtain 0.35 g (yield: 63%) of the title compound.

출처