HRID2082723

反应详情

EQUATION

反应方程式

HRID 2082723 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a cooled solution of sodium (8.2 g., 0.356 g-atom) in 300 ml. ethanol was added all at onece 2-ethoxybenzamidine hydrochloride (35.7 g., 0.178 mole). A solution of diethyl ethoxymethylenemalonate (38.4g., 0.178 mole) in 80 ml. of ethanol was added to the suspension and the mixture was heated under reflux for 21/4 hours. The cooled solution was added to about 2800 ml. of ice-water and the mixture was acidified to pH 5 with glacial acetic acid. The precipitated title product was dried to give 47 g. of an off-white solid, m.p. 147°-150°.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 21/4 hours
  3. additionThe cooled solution was added to about 2800 ml
  4. customThe precipitated title product
  5. customwas dried
  6. customto give 47 g