HRID63650

反应详情

EQUATION

反应方程式

HRID 63650 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-{3-[Methyl(phenyl)amino]phenyl}ethan-1-ol (1.0 g, 4.4 mmol) was stirred in 4N HCl/dioxane (8 mL) at 0° C. Aminoacetaldehyde diethyl acetal (880 mg, 6.6 mmol) was added, and the reaction stirred for at r.t. for 1 h and then at 108° C. in the microwave for 1 h. The solution was concentrated and purified by silica gel chromatography (0% to 20% MeOH/DCM) to give 150 mg (13%) of the title compound as a yellow oil. [M+H] Calc'd for C17H20N2O, 269. Found, 269.

WORKUP

后处理

  1. waitat 108° C. in the microwave for 1 h
  2. concentrationThe solution was concentrated
  3. custompurified by silica gel chromatography (0% to 20% MeOH/DCM)