HRID910117

反应详情

EQUATION

反应方程式

HRID 910117 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Add 2,4-dimethoxybenzylamine (27.64 g, 165.3 mmol) to a solution of indole-7-carboxaldehyde (20.0 g, 137.7 mmol) and acetic acid (8.26 ml, 137.7 mmol) in toluene (250 ml). Reflux and collect water using a Dean-Stark trap while replacing with fresh anhydrous toluene. Concentrate under reduced pressure, dissolve the residue in methanol and add sodium borohydride in portions. Dilute with ethyl acetate and wash sequentially with saturated aqueous sodium bicarbonate followed by saturated aqueous sodium chloride, dry over magnesium sulfate, and concentrate under reduced pressure to provide the desired compound as a brown oil.

WORKUP

后处理

  1. temperatureReflux
  2. customcollect water using a Dean-Stark trap
  3. concentrationConcentrate under reduced pressure
  4. dissolutiondissolve the residue in methanol
  5. additionadd sodium borohydride in portions
  6. additionDilute with ethyl acetate
  7. washwash sequentially with saturated aqueous sodium bicarbonate
  8. dry with materialdry over magnesium sulfate
  9. concentrationconcentrate under reduced pressure