乙氧基甲叉丙二酸二乙酯 → Diethyl 2-(((3-fluoro-4,5-dimethoxyphenyl)amino)methylene)malonate

HRID 525933笔记

反应方程式

HRID 525933 反应方程式
[F:1][C:2]1[CH:3]=[C:4]([CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10])[NH2:5].C(O[CH:16]=[C:17]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[C:18]([O:20][CH2:21][CH3:22])=[O:19])C>C(O)C>[F:1][C:2]1[CH:3]=[C:4]([NH:5][CH:16]=[C:17]([C:18]([O:20][CH2:21][CH3:22])=[O:19])[C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10]

参与物

4

反应物 2

HCID 6871乙氧基甲叉丙二酸二乙酯HCID 574295473-Fluoro-4,5-dimethoxyaniline

产物 1

HCID 86732800Diethyl 2-(((3-fluoro-4,5-dimethoxyphenyl)amino)methylene)malonate收率 98%

试剂、催化剂与溶剂 1

HCID 702乙醇溶剂

反应条件

温度
80 °C

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.

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

来源与证据

ORD记录
ord-105776c3b46443a2a7ea413fb9be6409
来源数据集
uspto-grants-2016_05
专利号
US09340556B2

反应笔记

加载中…