HRID1852976
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
- 50 °C
PROCEDURE
实验过程
7-(1-Methyl-1H-pyrazol-4-yl)-5-(1H-pyrazol-4-yl)imidazo[1,2-c]pyrimidine (Preparation K; 0.040 mg, 0.15 mmol) was dissolved in dimethylformamide (0.6 mL) and 5,5-dimethylhex-2-enenitrile (Table 1, compound k; 56 mg, 0.045 mmol) and 2,3,4,6,7,8,9,10-octahydropyrimido[1,2-a]azepine (34 mg, 0.23 mmol) were added and the reaction was heated at 50° C. for 7 hours. The reaction was then cooled and the solvent was removed. The crude reaction was purified by silica gel chromatography using a gradient (1 to 4% MeOH/DCM) to provide 3-(4-(7-(1-methyl-1H-pyrazol-4-yl)imidazo[1,2-c]pyrimidin-5-yl)-1H-pyrazol-1-yl)pentanedinitrile (37 mg, 63% yield) as a solid. MS (apci) m/z=389.2 (M+H).
WORKUP
后处理
- temperatureThe reaction was then cooled
- customthe solvent was removed
- customThe crude reaction
- customwas purified by silica gel chromatography