HRID554605

反应详情

EQUATION

反应方程式

HRID 554605 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 2-bromo-5-(trifluoromethyl)benzaldehyde (7.5 g, 29.6 mmol) in MeOH (80 mL) was added ethylamine (2M in MeOH; 30 mL, 60 mmol), sodium cyanoborohydride (3.7 g, 58.9 mmol), and acetic acid (1.7 mL, 26.2 mmol), and the reaction was stirred at room temperature for 4 days. The mixture was quenched with saturated aqueous NaHCO3 and extracted with CH2Cl2, and the combined organic layers were dried over MgSO4, filtered, and concentrated. The crude material was purified by silica gel chromatography (0-4% MeOH in CH2Cl2) to give (2-bromo-5-trifluoromethyl-benzyl)-ethyl-amine.

WORKUP

后处理

  1. customThe mixture was quenched with saturated aqueous NaHCO3
  2. extractionextracted with CH2Cl2
  3. dry with materialthe combined organic layers were dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe crude material was purified by silica gel chromatography (0-4% MeOH in CH2Cl2)