反应详情

6-[3-(Trifluoromethyl)phenyl]-4-pyridazinamine (2.0 g, 0.0084 mole, Compound No. 4) and N-chlorosuccinimide (0.61 g, 0.004 mole) were refluxed under N2 in CH3CN (50 mL) for 1.5 h. After this time no starting material was present by TLC. The mixture was partitioned between EtOAc/water. The organic layer was extracted again with water, dried (MgSO4), filtered and evaporated to give a crude oil. The oil was chromatographed on a Prep-500 using EtOAc/cyclohexane (9:1) to give a crude solid. The solid was recrystal-lized from EtOAc/cyclohexane to give 5-chloro-6-[3-(trifluoromethyl)phenyl]-4-pyridazinamine (0.57 g, 50% yield, Compound No. 35) as a tan solid.

1. customThe mixture was partitioned between EtOAc/water
2. extractionThe organic layer was extracted again with water
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. customevaporated
6. customto give a crude oil
7. customThe oil was chromatographed on a Prep-500 using EtOAc/cyclohexane (9:1)
8. customto give a crude solid