Water → 3-Iodopyridine-2,6-diamine

2,6-Diaminopyridine (100 g, 916 mmol) was dissolved in dimethyl sulfoxide (400 mL), and N-iodosuccinimide (100 g, 445 mmol) was added in one portion while stirring at room temperature. The reaction solution was stirring for 10 minutes at room temperature. Water (3.5 L) was added to the reaction solution, and the precipitated solids were filtered out. The resulting aqueous layer was extracted with ethyl acetate (1.3 L) 3 times. The ethyl acetate layers were combined and the solvent was evaporated under a reduced pressure. The residue was purified by silica gel chromatography (heptane:ethyl acetate=2:3) to obtain the title compound (23.8 g, 22.8%).

1. stirringThe reaction solution was stirring for 10 minutes at room temperature
2. filtrationthe precipitated solids were filtered out
3. extractionThe resulting aqueous layer was extracted with ethyl acetate (1.3 L) 3 times
4. customthe solvent was evaporated under a reduced pressure
5. customThe residue was purified by silica gel chromatography (heptane:ethyl acetate=2:3)

ORDレコード

ord-3aa85e0c537f40388de71e7309cd7eb1

出典データセット

uspto-grants-2014_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08841327B2