反应详情

3-Chloro-4-methoxy-6-[3-(trifluoromethyl)phenyl]pyridazine (2.0 g, 0.0069 mole, Compound No. 48) and sodium thiomethoxide (0.5 g, 0.0069 mole) were refluxed overnight under N2 in THF (50 mL). After this time no starting material was present by TLC. The mixture was partitioned between EtOAc-water. The aqueous layer was extracted again with EtOAc. The EtOAc layers were combined, washed with brine, dried (MgSO4), filtered and evaporated to give a crude oil. The oil was chromatographed on a Prep-500 using EtOAc-cyclohexane (3:17) to give 4-methoxy-3-(methylthio)-6-[3-(trifluoromethyl)phenyl]pyridazine (1.83 g, 88% yield, Compound No. 64) as a white solid.

1. customThe mixture was partitioned between EtOAc-water
2. extractionThe aqueous layer was extracted again with EtOAc
3. washwashed with brine
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customevaporated
7. customto give a crude oil
8. customThe oil was chromatographed on a Prep-500 using EtOAc-cyclohexane (3:17)