反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 35 °C
PROCEDURE
实验过程
To a solution of 1-(3-(1-(6-fluoro-1-methyl-1H-indazol-5-yl)ethyl)imidazo[1,2-b]pyridazin-6-yl)ethanone (35 mg, 0.104 mmol) in MeOH (4 mL), was added hydrazinecarboxamide hydrochloride (28.9 mg, 0.259 mmol). The reaction mixture was heated to 35° C. After stirring for 5 h, the solvent was removed and DCM was added to dilute the residue. The resulting mixture was then washed with brine, dried over Na2SO4, and concentrated in vacuo to give (E)-2-(1-(3-(1-(6-fluoro-1-methyl-1H-indazol-5-yl)ethyl)imidazo[1,2-b]pyridazin-6-yl)ethylidene)hydrazinecarboxamide (14 mg, 33%) as a white solid. 1H-NMR (400 MHz, DMSO-d6) δ ppm 9.64 (s, 1H), 8.14 (d, 1H), 7.93 (m, 2H), 7.74 (s, 1H), 7.51 (m, 2H), 4.93 (m, 1H), 3.96 (s, 3H), 2.13 (s, 3H), 1.76 (d, 3H). LCMS (method B): [MH]+=395, tR=2.32 min.
WORKUP
后处理
- customthe solvent was removed
- additionDCM was added
- additionto dilute the residue
- washThe resulting mixture was then washed with brine
- dry with materialdried over Na2SO4
- concentrationconcentrated in vacuo