HRID704504

反应详情

EQUATION

反应方程式

HRID 704504 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 4 liters of ethanol was suspended 45.4 g of 7-hydroxy-5-methoxycarbonyl-2-methyl-s-triazolo[1,5-a]pyrimidine and 37.83 g of sodium borohydride was added little by little thereto, and the mixture was then stirred at room temperature for 3 hours. A residue obtained by removing ethanol was dissolved in 2 liters of water, and 500 ml of Amberlite IRC-50 (H+) (trade name) was added thereto and stirred. Subsequently, the mixture was filtered and after removing water from the filtrate, 500 ml of methanol was added to the filtrate and the mixture was stirred. Then, methanol was removed from the mixture to obtain a residue. These procedures were repeated three times. Then, 500 ml of ethanol was added to the residue and the mixture was condensed. Precipitated crystals were collected by filtration, washed with ethanol and dried to obtain 39.35 g of the title compound.

WORKUP

后处理

  1. additionwas added little by little thereto, and the mixture
  2. customA residue obtained
  3. customby removing ethanol
  4. dissolutionwas dissolved in 2 liters of water
  5. addition500 ml of Amberlite IRC-50 (H+) (trade name) was added
  6. stirringstirred
  7. filtrationSubsequently, the mixture was filtered
  8. customafter removing water from the filtrate, 500 ml of methanol
  9. additionwas added to the filtrate
  10. stirringthe mixture was stirred
  11. customThen, methanol was removed from the mixture
  12. customto obtain a residue
  13. customcondensed
  14. customPrecipitated crystals
  15. filtrationwere collected by filtration
  16. washwashed with ethanol
  17. customdried