HRID2080115

反应详情

EQUATION

反应方程式

HRID 2080115 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-Ethoxymethylene-malonic acid diethyl ester (5.00 g, 23.1 mmol), hydroxylamine hydrochloride (4.01 g, 57.8 mmol) and triethylamine (8.06 mL, 57.8 mmol) were dissolved in ethanol (100 mL), the solution was stirred at room temperature for 17 hours, then, the solution was stirred for 4.5 hours under reflux. The reaction solution was cooled to room temperature, water was added, and 1N hydrochloric acid was added until a salt precipitated. The precipitated salt was collected by filtration, and a hydrochloride salt of the title compound (2.39 g, 15.2 mmol, 66%) was obtained as a white solid.

WORKUP

后处理

  1. stirringthe solution was stirred for 4.5 hours
  2. temperatureunder reflux
  3. temperatureThe reaction solution was cooled to room temperature
  4. customprecipitated
  5. filtrationThe precipitated salt was collected by filtration