HRID1703731

反应详情

EQUATION

反应方程式

HRID 1703731 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-cyano-1-(2,3,5-tri-O-acetyl-β -D-ribofuranosyl)-1,2,4-triazole (8.0 g., 22.7 mmole), triethylamine (14.0 ml.) and ethanol (200 ml.) was stirred at 25° while hydrogen sulfide gas was passed into the solution for 2 hrs. The solvent was removed and the residue was treated with a solution of sodium methoxide (600 mg.) in methanol (150 ml.) for three hours at 25°. After the solution was neutralized with Bio-Rad AG 50W-X2(H), it as filtered, and the solvent was removed. Crystallization of the product from aqueous ethanol provided 4.5 g. (76.0%) of the thiocarboxamide with M.P. 173-175°.

WORKUP

后处理

  1. customThe solvent was removed
  2. additionthe residue was treated with a solution of sodium methoxide (600 mg.) in methanol (150 ml.) for three hours at 25°
  3. filtrationit as filtered
  4. customthe solvent was removed
  5. customCrystallization of the product from aqueous ethanol
  6. customprovided 4.5 g