Sodium Carbonate → 4-(4-Pyridyl)-2-butanone oxime

Next, water (12 ml) and tetrahydrofuran (1.2 ml) were added to 4-(4-pyridyl)-2-butanone (736 mg, 3.96 mmol), and the mixture was stirred at room temperature. Sodium carbonate (483 mg, 4.56 mmol) and hydroxylamine hydrochloride (358 mg, 5.15 mmol) were added to the mixture, the whole was stirred for 1.5 hours, and then ethyl acetate (50 ml) was added to the reaction mixture to dilute it. Sodium hydrogencarbonate was added thereto. After separation, the organic layer was washed with saturated brine (10 ml), dried over anhydrous sodium sulfate and concentrated under reduced pressure. Cyclohexane was added to the resulting crystals, and the crystals were filtered off to give 4-(4-pyridyl)-2-butanone oxime (584 mg, 90%) as pale yellow crystals.

1. stirringthe whole was stirred for 1.5 hours
2. additionto dilute it
3. customAfter separation
4. washthe organic layer was washed with saturated brine (10 ml)
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated under reduced pressure
7. additionCyclohexane was added to the resulting crystals
8. filtrationthe crystals were filtered off

ORD-Eintrag

ord-a2942a5370974c94897ea627c6c2929b

Quelldatensatz

uspto-grants-2010_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07741346B2