HRID614326

反应详情

EQUATION

反应方程式

HRID 614326 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 75 g of 7-(3-aminopropyl)-theophylline and 27.4 g of 1-chloro-3-phenoxy-2-propanol is heated for 8 hours at 130° to 140° C. After the melt has been cooled to 70°-90° C., ethanol is added to it, followed by brief boiling under reflux. After standing overnight, the untreated and precipitated aminopropyl theophylline hydrochloride is filtered off under suction, the filtrate is acidified with alcoholic hydrochloric acid, heavily concentrated and acetone added until crystallisation begins. The reaction product then separates and is recrystallised from methanol. Yield 30.2 g. Melting point of the hydrochloride: 183°-186° C.

WORKUP

后处理

  1. temperatureis heated for 8 hours at 130° to 140° C
  2. temperatureAfter the melt has been cooled to 70°-90° C.
  3. temperatureunder reflux
  4. customthe untreated and precipitated aminopropyl theophylline hydrochloride
  5. filtrationis filtered off under suction
  6. concentrationheavily concentrated
  7. additionacetone added until crystallisation
  8. customis recrystallised from methanol
  9. custom183°-186° C.