Hydrogen Peroxide → HCID 137231110, compound

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.

1. additionwere added, at room temperature
2. distillationThe solvent was distilled off under reduced pressure
3. additionWater was added to the residue and extraction with ethyl acetate
4. washThe organic layer was washed with a saturated aqueous sodium chloride solution
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationfiltered
7. customto remove inorganic matter
8. distillationThe solvent was distilled off under reduced pressure
9. washThe resulting crude crystal was washed with a 1:2 mixed solution of diisopropyl ether and n-hexane

ORD record

ord-58b0274909c14fdcad918bf857f37136

Source dataset

uspto-grants-2015_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09044013B2