Ammonium Chloride → 453565-59-8

Temperature

90 °C

3-Iodobenzonitrile (7.00 g, 30.6 mmol) was dissolved in ethanol (153 mL), and the mixture was stirred at 90° C. for 2 hours after adding hydroxylamine hydrochloride (4.30 g, 61.2 mmol) and N,N-diisopropylethylamine (10.5 mL, 61.2 mmol). After adding an aqueous ammonium chloride solution, insoluble were separated by filtration through sellite. The organic layer of the filtrate was separated, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was then purified by silica gel column chromatography to give N′-hydroxy-3-iodobenzamidine (8.37 g, quantitative).

1. custominsoluble were separated by filtration through sellite
2. customThe organic layer of the filtrate was separated
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe residue was then purified by silica gel column chromatography

ORD record

ord-222332d45ff646608b25752bd8a64534

Source dataset

uspto-grants-2011_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07998954B2