反应详情

Trifluoroacetic acid (30 mL) was added to a solution of (5-bromo-6-chloro-4-iodo-pyridin-3-yl)-carbamic acid tert-butyl ester (19.0 g, 44 mmol) in DCM (120 mL) and the resultant solution was stirred at ambient temperature for 2 h then concentrated in vacuo. The resultant residue was loaded onto an SCX-2 cartridge (70 g) eluting with acetonitrile (100 mL) then 2N ammonia in methanol (100 mL). The basic fraction was concentrated in vacuo to afford the title compound (11.5 g, 78%). 1H NMR (DMSO-D6, 400 MHz): 7.23 (s, 1H), 5.92 (s, 2H).

1. concentrationthen concentrated in vacuo
2. washeluting with acetonitrile (100 mL)
3. concentrationThe basic fraction was concentrated in vacuo