HRID900240

反应详情

EQUATION

反应方程式

HRID 900240 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
190 °C

PROCEDURE

实验过程

1.0 g (5.9 mmol) of 4-chloro-N-hydroxy-benzamidine and 776 mg (7.96 mmol) of propynoic acid ethyl ester were dissolved in methanol and the resulting solution was boiled under reflux for 15 h. The solvent was removed under reduced pressure, and the residue was dissolved in Dowtherm A. This solution was heated to 190° C. for 2.5 h, allowed to cool, then poured into n-heptane. The precipitated product was filtered off and washed with n-heptane.

WORKUP

后处理

  1. temperatureunder reflux for 15 h
  2. customThe solvent was removed under reduced pressure
  3. dissolutionthe residue was dissolved in Dowtherm A
  4. temperatureto cool
  5. additionpoured into n-heptane
  6. filtrationThe precipitated product was filtered off
  7. washwashed with n-heptane