HRID1449526

反应详情

EQUATION

反应方程式

HRID 1449526 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 30 ml of ethanol was dissolved 750 mg of N-[4-(5-ethoxycarbonyl-pentylthio)phenyl]-3-propyl-6,7-dihydro-5H-thiazolo[3,2-a]pyrimidine-2-carboxamide hydrochloride obtained in Example 89. To the solution was added 3.22 ml of 1N sodium hydroxide aqueous solution, followed by reflux under heating for 2 hours. After cooling the mixture, ethanol was removed under reduced pressure. The aqueous solution was made acidic with consentrated hydrochloric acid, following by removing a little amount of water. To the residue was added isopropylalcohol-diethylether and the precipitated crystals were collected by filtration. This crystals were recrystallized from methanol-diethylether to obtain 494 mg of the titled compound.

WORKUP

后处理

  1. temperatureby reflux
  2. temperatureunder heating for 2 hours
  3. customwas removed under reduced pressure
  4. customby removing a little amount of water
  5. additionTo the residue was added isopropylalcohol-diethylether
  6. filtrationthe precipitated crystals were collected by filtration
  7. customThis crystals were recrystallized from methanol-diethylether