反应详情

A solution of 2-(3-methoxyquinolin-6-yl)-2-methyl-N′-(6-phenylpyridazin-3-yl)propanehydrazide (270 mg, 653 μmol) in TFA (2 mL) was heated to 150° C. in microwave (6 bar; 20 W) for 2 h. LCMS suggests very good conversion: 89425-17-1. Reaction concentrated under reduced pressure then partitioned between CHCl3/IPA (50 mL) and 1M NaOH (50 mL). Aqueous further extracted with CHCl3/IPA (15 mL) and combined organics dried over MgSO4, concentrated, then dissolved in ACN (2 mL). Crystallized solid washed with ACN (1 mL) and dried under reduced pressure. MS (ESI pos. ion) m/z: 396 (MH+). Calc'd exact mass for C24H21N5O: 395.

1. customReaction
2. concentrationconcentrated under reduced pressure
3. customthen partitioned between CHCl3/IPA (50 mL) and 1M NaOH (50 mL)
4. extractionAqueous further extracted with CHCl3/IPA (15 mL)
5. dry with materialcombined organics dried over MgSO4
6. concentrationconcentrated
7. dissolutiondissolved in ACN (2 mL)
8. customCrystallized solid
9. washwashed with ACN (1 mL)
10. customdried under reduced pressure