HRID525933

反应详情

EQUATION

反应方程式

HRID 525933 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To the suspension of 3-fluoro-4,5-dimethoxyaniline (73 g, 426 mmol) in Ethanol (100 mL) was added diethyl 2-(ethoxymethylene)malonate (85 mL, 426 mmol), and the resulting mixture was heated at 80° C. for 1 h. LCMS indicated completion of the reaction. The mixture was concentrated in vacuo to remove ethanol, and the residue was washed with hexane to afford diethyl 2-(((3-fluoro-4,5-dimethoxyphenyl)amino)methylene)malonate (142 g, 416 mmol, 98% yield) as a yellow solid. LCMS: (M+H)+: 342.1.

WORKUP

后处理

  1. customcompletion of the reaction
  2. concentrationThe mixture was concentrated in vacuo
  3. customto remove ethanol
  4. washthe residue was washed with hexane