反应详情

N-(3-iodo-5-(trifluoromethyl)pyridin-2-yl)pivalamide (16.8 g, 45.1 mmole) was taken up in H2SO4 (24 wt. %, 392 ml) and the mixture was stirred for 60 minutes under reflux. After cooling to RT the mixture was neutralised with 4 N NaOH and solid NaHCO3, the aqueous phase was extracted with DCM (3×200 ml) and the combined organic phases were dried over MgSO4. After filtration the solvent was removed on a rotary evaporator. 3-iodo-5-(trifluoromethyl)pyridin-2-amine (13 g, 100%) was obtained as a cream-coloured solid.

1. temperatureunder reflux
2. extractionthe aqueous phase was extracted with DCM (3×200 ml)
3. dry with materialthe combined organic phases were dried over MgSO4
4. filtrationAfter filtration the solvent
5. customwas removed on a rotary evaporator