HRID1465752

反应详情

EQUATION

反应方程式

HRID 1465752 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

To a flask containing a stir bar was added 7-Bromo-3-chloro-8-methylisoquinoline (0.63 g, 2.4 mmol), CuCN (0.33 g, 3.7 mmol), and DMF (10 mL). The mixture was then refluxed at 150° C. overnight. When the reaction was complete, as evidenced by LC analysis, the reaction flask was taken out of the oil bath and cooled to room temperature. To the mixture was then poured DCM (20 mL) and a precipitate formed immediately, which was filtered, re-dissolved in DCM, adsorbed into silica gel and purified by silica gel column chromatography (Hexanes:DCM→1:1) to provide the title product. LC/MS (IE, m/z): [M+1]+=203.

WORKUP

后处理

  1. additionTo a flask containing a stir bar
  2. temperaturecooled to room temperature
  3. filtrationwhich was filtered
  4. dissolutionre-dissolved in DCM
  5. custompurified by silica gel column chromatography (Hexanes:DCM→1:1)