HRID1454937

反应详情

EQUATION

反应方程式

HRID 1454937 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

Under argon, benzaldehyde (584 μl, 5.75 mmol) is added to a solution of 8-amino-4-bromoisoquinoline (Intermediate 23.2, 1.11 g, 5 mmol) in absolute EtOH (60 ml). The mixture is heated at 90° C. for 24 h. It is cooled to 0° C. and then sodium cyanoborohydride (NaBH3CN, 3.3 g, 50 mmol) is added in small portions. The stirring is maintained for 2 h at room temperature. The reaction mixture is diluted with AcOEt (600 ml) and is then washed with water. The organic phase is dried over Na2SO4 and then evaporated. The residue is purified on silica gel, eluting with an AcOEt/petroleum ether (1/4) mixture.

WORKUP

后处理

  1. temperatureIt is cooled to 0° C.
  2. temperatureThe stirring is maintained for 2 h at room temperature
  3. washis then washed with water
  4. dry with materialThe organic phase is dried over Na2SO4
  5. customevaporated
  6. customThe residue is purified on silica gel
  7. washeluting with an AcOEt/petroleum ether (1/4) mixture