反应详情

温度

60 °C

5-Bromo-4-methyl-3-(3-trifluoromethyl-phenyl)-pyridin-2-ylamine (Int. 1, 12.0 g, 36.25 mmol) was stirred in dioxane (250 mL) at RT and ethoxycarbonyl isothiocyanate (4.27 mL, 36.25 mmol) was added dropwise. The reaction mixture was stirred for 18 hrs, then the solvent was evaporated in vacuo. The resultant residue was dissolved in MeOH/IMS (1:1, 460 mL) and hydroxylamine hydrochloride (12.58 g, 181 mmol) was added and the reaction mixture was heated to 60° C. DIPEA (18.6 mL, 109 mmol) was added, and the reaction mixture was heated for a further 4.5 rs before allowing to cool. The resultant precipitate was collected by filtration, washed with MeOH and dried to afford the title compound as a white solid (11.49 g).

1. customthe solvent was evaporated in vacuo
2. dissolutionThe resultant residue was dissolved in MeOH/IMS (1:1, 460 mL)
3. temperaturethe reaction mixture was heated for a further 4.5 rs
4. temperatureto cool
5. filtrationThe resultant precipitate was collected by filtration
6. washwashed with MeOH
7. customdried