Water → 3-Iodopyridine-2,6-diamine

2,6-Diaminopyridine (100 g) was dissolved in DMSO (400 mL), and N-iodosuccinimide (100 g) was added thereto all at once under stirring at room temperature. The reaction solution was stirred for 10 minutes at room temperature, after which water (3.5 L) was added thereto and the precipitated solids were filtered off. The aqueous layer thus obtained was extracted with ethyl acetate (1.3 L) 3 times. The ethyl acetate layers were combined, and which was concentrated under a reduced pressure, and the residue thus obtained was purified by silica gel chromatography (heptane:ethyl acetate=2:3) to obtain the titled compound (24 g).

1. stirringThe reaction solution was stirred for 10 minutes at room temperature
2. filtrationthe precipitated solids were filtered off
3. customThe aqueous layer thus obtained
4. extractionwas extracted with ethyl acetate (1.3 L) 3 times
5. concentrationwhich was concentrated under a reduced pressure
6. customthe residue thus obtained
7. customwas purified by silica gel chromatography (heptane:ethyl acetate=2:3)

ORD record

ord-19efe85b1e8541f4b78299a256290baf

Source dataset

uspto-grants-2012_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08183264B2