6-Bromo-N-(tert-butyl)-3-methylpyridin-2-amine → 6-Bromo-3-methylpyridin-2-amine

A solution of (6-bromo-3-methylpyridin-2-yl)-tert-butylamine (500 mg, 2.06 mmol) in DCE (2 mL) and TFA (2 mL) was heated at 120° C. for 10 min in a microwave reactor, and then concentrated under reduced pressure. The residue was taken up in MeOH and loaded onto an Isolute® SCX-2 cartridge (10 g). The cartridge was washed with MeOH then the desired product eluted with 2 M NH3 in MeOH to give 6-Bromo-3-methylpyridin-2-ylamine as a white solid (359 mg, 93%). 1H NMR (400 MHz, CHCl3-d): δ 7.11 (d, J=7.5 Hz, 1 H); 6.77 (d, J=7.5 Hz, 1 H); 4.50 (s, 2 H); 2.07 (s, 3 H).

1. concentrationconcentrated under reduced pressure
2. washThe cartridge was washed with MeOH
3. washthe desired product eluted with 2 M NH3 in MeOH

ORD record

ord-67b6356acce74df9a28cb34bff4de5c3

Source dataset

uspto-grants-2013_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08394796B2