HRID1503201

反应详情

EQUATION

反应方程式

HRID 1503201 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7.8 g (60 mmol) of 2-nitroiminoimidazolidine and 12.1 g (87.5 mmol) of potassium carbonate were dissolved in 60 ml of acetonitrile in a reflux flask. The mixture is heated to a temperature sufficient for achieving reflux operating condition. 8.1 g (50.0 mole) of 2-chloro-5-chloromethyl pyridine is dissolved in 40 ml of acetonitrile, and is dropwisely and continuously added into the flask under the reflux condition for a period of 0.5 hr, i.e. the addition rate is about 1.5 ml/minute (the addition rate at the onset of the reaction corresponds to 0.0278 equivalent of 2-chloro-5-chloromethyl pyridine per equivalent of 2-nitroiminoimidazolidine per minute) After completion of the reaction, the mixture is subjected to filtration. The filtrate is concentrated, and is further purified.

WORKUP

后处理

  1. temperatureThe mixture is heated to a temperature sufficient
  2. temperaturefor achieving reflux
  3. additioncontinuously added into the flask under the reflux condition for a period of 0.5 hr
  4. customAfter completion of the reaction
  5. filtrationthe mixture is subjected to filtration
  6. concentrationThe filtrate is concentrated