HRID1634549

反应详情

EQUATION

反应方程式

HRID 1634549 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Treat a solution of N-(2-amino-ethyl)-2-(4-ethoxy-3-methoxy-phenyl)acetamide (0.7 g, 2.77 mmol) in THF (10 mL) with AlH3.NMe2Et (55 mL, 27.74 mmol) and heat to reflux for 14 h. Cool the resulting mixture to ambient temperature, quench with Na2CO3.10H2O (0.5 g) and stir at ambient temperature for 15 min. Filter the solution through Celite and wash with several portions of CH2Cl2. Concentrate the filtrate in vacuoo and purify by preparative TLC (10% MeOH in CH2Cl2) to obtain the title compound as a white oil.

WORKUP

后处理

  1. temperatureto reflux for 14 h
  2. customquench with Na2CO3.10H2O (0.5 g)
  3. filtrationFilter the solution through Celite
  4. washwash with several portions of CH2Cl2
  5. concentrationConcentrate the filtrate in vacuoo
  6. custompurify by preparative TLC (10% MeOH in CH2Cl2)