HRID614239

反应详情

EQUATION

反应方程式

HRID 614239 的结构方程式

PROCEDURE

实验过程

3-Carbamoyl-4-(p-methoxybenzyl)-1,2,4-triazole-5-thiol (2.0 g., 0.007 mole), trifluoroacetic acid (8 ml.) and anisole (2 ml.) were heated at 70° C. for 3.5 hours. At this point, most of the trifluoroacetic acid present was removed by means of evaporation under reduced pressure and the residue was subsequently triturated with diethyl ether. The resulting solid was then filtered, washed with diethyl ether and subsequently dried in vacuo at 50° C. to give pure 3-carbamoyl-1,2,4-triazole-5-thiol (1.0 g., 91% yield), m.p. 276°-278° C. The infrared absorption spectrum was identical to that of a reference sample prepared as described in Example XVI, Part C.

WORKUP

后处理

  1. customAt this point, most of the trifluoroacetic acid present was removed by means of evaporation under reduced pressure
  2. customthe residue was subsequently triturated with diethyl ether
  3. filtrationThe resulting solid was then filtered
  4. washwashed with diethyl ether
  5. customsubsequently dried in vacuo at 50° C.