反应详情

温度

5 °C

(4-Methoxy-benzyl)-[4-trifluoromethyl-6-(4-trifluoromethyl-phenyl)-pyridazin-3-yl]-amine (example C.26 step 8) (6.48 g, 15 mmol) was added portionwise at 5° C. to conc. H2SO4 (d 1.83, 17.0 mL, 303 mmol). The deep purple solution was stirred for 5 min at 5° C. then the cooling bath was removed and stirring was continued for further 60 min at 23° C. The mixture was poured onto ice, made alkaline with 32% NaOH-sol., saturated with solid NaCl and extracted with THF and TBME, dried the organic layer over MgSO4. Removal of the solvent in vacuum left the title compound as a light yellow solid (4.44 g, 95%), which was used without further purification. MS (ISP) 308.1 [(M+H)+]; mp 186-190° C.

1. customthe cooling bath was removed
2. stirringstirring
3. waitwas continued for further 60 min at 23° C
4. additionThe mixture was poured onto ice
5. extraction, saturated with solid NaCl and extracted with THF and TBME
6. dry with materialdried the organic layer over MgSO4
7. customRemoval of the solvent in vacuum
8. waitleft the title compound as a light yellow solid (4.44 g, 95%), which
9. customwas used without further purification