HRID1852976

反应详情

EQUATION

反应方程式

HRID 1852976 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe reaction was then cooled
  2. customthe solvent was removed
  3. customThe crude reaction
  4. customwas purified by silica gel chromatography