HRID1032571

反应详情

EQUATION

反应方程式

HRID 1032571 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 400 ml of ethanol was dissolved 23.7 g of 2-acetoxymethyl-7-chloro-5-methyl-s-triazolo[1,5-a]pyrimidine, and 19 g of thiourea was added thereto and the mixture was stirred for 30 minutes under reflux. The reaction mixture was ice-cooled and the precipitated crystals were collected by filtration, washed with ethanol and dried. After the obtained crystals were dissolved in a 10% potassium hydroxide aqueous solution and stirred for 30 minutes, pH was adjusted to 2 with addition of a 2N hydrochloric acid. The precipitated crystals were collected by filtration, washed with water and dried to obtain 15.3 g of the title compound.

WORKUP

后处理

  1. additionwas added
  2. temperatureunder reflux
  3. temperaturecooled
  4. filtrationthe precipitated crystals were collected by filtration
  5. washwashed with ethanol
  6. customdried
  7. dissolutionAfter the obtained crystals were dissolved in a 10% potassium hydroxide aqueous solution
  8. stirringstirred for 30 minutes
  9. additionpH was adjusted to 2 with addition of a 2N hydrochloric acid
  10. filtrationThe precipitated crystals were collected by filtration
  11. washwashed with water
  12. customdried