HRID127140

反应详情

EQUATION

反应方程式

HRID 127140 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Amino-5-[N-(1-ethylpropyl)aminosulfonyl]-1,3,4-thiadiazole (0.10 mole) and xylene (200 ml) are charged into a glass reaction vessel fitted with a mechanical stirrer, thermometer and condenser. The mixture is dried by azeotroping off water and is then cooled to room temperature. Oxalyl chloride (0.15 mole) is added; the reaction mixture is warmed to a temperature of from 80° C. to about 100° C. and stirred at this temperature for a period of about 1 hour. The mixture is then heated to reflux and stirred for an additional 2 hours. Solvent is then stripped off leaving the desired product 5-[N-(1-ethylpropyl)aminosulfonyl]-1,3,4-thiadiazol-2-yl isocyanate dimer as the residue.

WORKUP

后处理

  1. customfitted with a mechanical stirrer
  2. customThe mixture is dried
  3. customby azeotroping off water
  4. temperaturethe reaction mixture is warmed to a temperature of from 80° C. to about 100° C.
  5. temperatureThe mixture is then heated
  6. temperatureto reflux
  7. stirringstirred for an additional 2 hours