HRID1853088

反应详情

EQUATION

反应方程式

HRID 1853088 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7-(1-Methyl-1H-pyrazol-4-yl)-5-(1H-pyrazol-4-yl)imidazo[1,2-c]pyrimidine (Preparation K-1; 0.050 g, 0.189 mmol), 2-(spiro[3.3]heptan-2-ylidene)acetonitrile (0.050 g, 0.377 mmol) and 2,3,4,6,7,8,9,10-octahydropyrimido[1,2-a]azepine (0.014 mL, 0.094 mmol) were suspended in MeCN (3 mL) and stirred at ambient temperature overnight. The reaction mixture was concentrated under reduced pressure and the crude material purified by flash column chromatography, eluting with 1-4% (9:1 MeOH:NH4OH)/DCM to provide 2-(2-(4-(7-(1-methyl-1H-pyrazol-4-yl)imidazo[1,2-c]pyrimidin-5-yl)-1H-pyrazol-1-yl)spiro[3.3]heptan-2-yl)acetonitrile (0.032 g, 0.080 mmol, 42% yield). MS (apci) m/z=399.2 (M+H).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe crude material purified by flash column chromatography
  3. washeluting with 1-4% (9:1 MeOH:NH4OH)/DCM