3-Aminopyridine → 1-(Pyridin-3-yl)piperazine

Temperature

140 °C

A suspension of 3-aminopyridine (2.0 g) and bis(2-chloroethyl)amine hydrochloride (3.8 g) in o-xylene (40 ml) was stirred at 140° C. for 20 hr. The reaction mixture was extracted with water and the aqueous layer was made alkaline with a 2N aqueous sodium hydroxide solution and extracted with chloroform. The extract was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated and the obtained residue was purified by silica gel column chromatography (developing solvent; chloroform:methanol:aqueous amnmonia=9:1:0.5) to give the title compound (0.55 g) as a black brown oil.

1. extractionThe reaction mixture was extracted with water
2. extractionextracted with chloroform
3. washThe extract was washed with saturated brine
4. dry with materialdried over anhydrous sodium sulfate
5. customThe solvent was evaporated
6. customthe obtained residue was purified by silica gel column chromatography (developing solvent; chloroform:methanol:aqueous amnmonia=9:1:0.5)

ORD record

ord-dda8921199984c88a1caa015b2aed9f5

Source dataset

uspto-grants-2002_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06455528B1