反应详情

A solution of N′-(6-chloropyridazin-3-yl)-2-(quinolin-6-yl)propanehydrazide (4300 mg, 13119 μmol) in TFA (40 mL) was heated to 120° C. with microwaves for 40 min. LCMS suggests very good converson. Solvents removed under reduced pressure and residue partitioned between 9:1 CHCl3/IPA (75 mL) and 1M NaOH (100 mL). Aqueous further extracted with 9:1 CHCl3/IPA (2×25 mL). Combined organics dried over MgSO4, concentrated, and oily residue dissolved in ACN/MeOH (2 mL). Resulting solid after 2 h was isolated by filtration and washed with ACN (5 mL). 6-(1-(6-chloro-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)ethyl)quinoline isolated as a white solid. MS (ESI pos. ion) m/z: 310 (MH+). Calc'd exact mass for C16H12ClN5: 309.

1. customSolvents removed under reduced pressure and residue
2. custompartitioned between 9:1 CHCl3/IPA (75 mL) and 1M NaOH (100 mL)
3. extractionAqueous further extracted with 9:1 CHCl3/IPA (2×25 mL)
4. dry with materialCombined organics dried over MgSO4
5. concentrationconcentrated
6. dissolutionoily residue dissolved in ACN/MeOH (2 mL)
7. customResulting solid after 2 h
8. customwas isolated by filtration
9. washwashed with ACN (5 mL)